Silk Road forums
Discussion => Off topic => Topic started by: Dopeboy on March 07, 2012, 10:50 am
-
Equipment:
* Hotplate/Stirrer
* magnetic stir bar
* Several five-gallon buckets
* Scales
* Several large beakers
* 2000ml flask
* Thermometer
* Large metal pot
* [Distillation setup if done indoors]
* Separatory funnel
* pH strips
* pyrex glass baking dish
Chemicals:
* alpha-methyl-3,4-(methylenedioxy)hydrocinnamaldehyde [CAS#1205-17-0]
* hydroxylamine hydrochloride
* nickel acetate
* methanol [or ethanol can be used]
* sodium carbonate
* sodium hydroxide
* household bleach
* xylene
* hydrochloric acid
* acetone
ALDEHYDE --> OXIME
1000g of substrate and 2000ml of methanol are added to a 5 gallon pail and stirred with a magnetic stirrer.
http://xfq5l5p4g3eyrct7.onion/upload/6e0730248a7caa8f7bb1269f778acb9c.jpg
700g of hydroxylamine hcl is dissolved in 1000g of water in a large beaker and is then added to the 5 gallon pail while stirring.
http://xfq5l5p4g3eyrct7.onion/upload/1cc44f915ecd40caff90ec42561a53b6.jpg
400g sodium carbonate is dissolved in 1000g of water in a separate beaker and allowed to cool for several hours in a sink full of cold water. The cooled solution is then added in 200-300ml portions slowly into the pail over a period of 2-3 hours with constant stirring. The solution should turn to a frothy green color. Stir for 12 hours and a solid mass should form at the bottom of the bucket. [If it does not solidify, mix another 350g of hydroxylamine hcl with 500g water and add this to the reaction, then add another 1000ml methanol and stir for another 12 hours].
http://xfq5l5p4g3eyrct7.onion/upload/38572fb5bc9e0ebe69f506ecff698f97.jpg
Filter out the solid and wash it thoroughly with water and let it dry.
http://xfq5l5p4g3eyrct7.onion/upload/6892ce57754bc1037d3468fea9cfa194.jpg
OXIME --> AMIDE
300g of the dried product is added to a 2000ml flask along with 900ml xylene and 6g nickel acetate.
http://xfq5l5p4g3eyrct7.onion/upload/025ff23454e00b0006e37bc99bc088ff.jpg
This mixture is heated to 130C for 6 hours. Distill or boil off 300-400ml of the xylene and allow it to cool for 12 hours until it solidifies.
http://xfq5l5p4g3eyrct7.onion/upload/63a5cdefc59770b428221a5d7bbe281e.jpg
Recrystallize the product with hot xylene [or boiling water]. Dry the recrystallized product and grind in into an extremely fine dust in a coffee grinder. It is very important that is a very fine dust with small particle size.
http://xfq5l5p4g3eyrct7.onion/upload/43ed083b3712d2bcf267a8e837c0ddee.jpg
AMIDE --> AMINE
Add 2000ml water and 1200ml bleach into a clean 4-liter plastic milk jug. Add 100g sodium hydroxide and shake it up well. Cool it in a fridge for several hours. Add 100g of the finely powdered product from the previous step to the milk jug. Shake this mixture up and place it in the fridge for 72 hours, shaking it every few hours [or as much as possible as often as possible]. Take it out of the fridge and let if sit at room temp for 24 hours, again shaking it up whenever you get the chance. Then place it in a hot water bath for 6-12 hours. It should be a milky orange color with tarry MDA base floating in it. Use a separatory funnel to extract the MDA base with xylene or toluene and discard the water layer. Next add diluted HCl acid until the pH of the water layer is 1 and discard the oil layer this time. Evaporate the acidified water layer in a pyrex baking tray. A kilo of the original substrate will yield about 250g of MDA.
http://xfq5l5p4g3eyrct7.onion/upload/41b65ce3728efeaaa9151285d87b1e22.jpg
Wash with acetone, using a metal putty/plaster knife to scrape and crush everything up.
http://xfq5l5p4g3eyrct7.onion/upload/7d306e92c74e14d9462d4c169cb7cae9.jpg
Recrystallize with acetone and water or your preferred method.
http://xfq5l5p4g3eyrct7.onion/upload/998334caefb178868ac6cf1c1623f7a4.jpg
A kilo of the original substrate will yield about 250g of MDA.
Original topic and discussion can be found at psychonaut.com
http://psychonaut.com/post-34173.html?f=43
-
I wont be buying any of that shit with my paypal account though!
-
Very interesting, I may have to make this a Summer project of mine. Since I'm too lazy at the moment can you give a rough estimate of the cost of all supplies?
-
Thanks for this interesting read!
Are you interested in writing some e-books?
Every synthase book on Sr is for chemicals, but I would be happy to have more books for stupids.
A lot of pictures and a step by step tutorial!
Easy synthase books on Sr: Cocaine_extraction,
whatchas-easy-mhrb-stb-extraction-_DIY,
amphetamine_Sulfate_pictorial__synthesis´
heroin manufacturing process
I think a lot of people would buy more good books..
-
Thanks for the read and info.
-
Have you done this dope boy? Some of those chemicals are watched, I assume you just count on getting lucky coming through customs to a PO box that isn't yours? What are the hardest parts? Why are more people not doing this and selling it as MDMA/MDA, is it profitable?
-
Everybody at this site should be setting up labs in their homes. And this is the perfect synthesis to get started with this hobby due to it's simplicity and none of the chemicals are very watched. The more people who get involved with chemistry as a hobby, the less they'll be able to persecute us. Just don't talk about it, keep it to yourself. Ignore the cops and government propaganda, they are just using fear and intimidation to control you, just like any corrupt regime. Ignore them just like you ignore internet trolls, even speaking to them gives them power.
As far as profits go... $500 for 250g of MDA you tell me if it's profitable. ;)
And I don't know how to do the ebook thing, but I'll look into it. If somebody has the time and know-how they should put this into pdf format and distribute it far and wide, all over the net. We need as many people as possible to become disobedient towards governments worldwide, and the next 4 years will be crucial.
laboyglass.com has get glassware for those who are interested.
-
dope boy you kick ass! when will you have listings again? your mdma was fire! turning 500 into 20,000+ is a dream that seems possible
-
Trust me if an ADHD learning impaired dummy like me can do it, ANYONE can.
-
fuck ebay. fuck paypal.. they froze my account
-
I like the idea, for sure more people should be cooking at home but aside from the dangers of dodgy product, won't the corrupt government just ban alpha-methyl-3,4-(methylenedioxy)hydrocinnamaldehyde or make it availible only under license? I suppose you'll just have to find another chem that isn't so restricted and work from there at that point....
-
is that how you made your MDA that was for sell on silk road dopeboy?
-
Sounds like an interesting project
-
is that how you made your MDA that was for sell on silk road dopeboy?
Yes it is.
-
an excellent and very interesting post, wish i had the balls and the faith in myself to actually give it a go but i dont, so i just make do with the theory
-
nice. have you tried that helional route? if so what were the yields?
guess i wont be getting in on the mda game soon lol but maybe synthetic mescaline, seems easy enough
Edit - also when are you restocking mdma again? cleanest product on SR :)
-
nice. have you tried that helional route? if so what were the yields?
guess i wont be getting in on the mda game soon lol but maybe synthetic mescaline, seems easy enough
Edit - also when are you restocking mdma again? cleanest product on SR :)
This IS the helional/floramelon route.
Edit: 25% yield for this is horrible btw, you could pull a lot more if you didn't cut so many corners.
-
whoops didnt read through the whole post and the different name caught me off guard lol
-
Totally missed this-
I was asked to come up with a synthesis for someone back in November, they linked me to some bullshit discussion on hipforums where the synth involved used sodium azide. After some lit searching and going back through some experiments I did in 2009, I pretty much came up with the same route, the only difference being I advised them to use Nickel Chloride (at a higher loading), 1.0M hypochlorite solution and potassium carbonate.
Didn't realise a similar prep was already available, I charged them 15BTC for my efforts :-[
-
Also, it would be good if a vendor could list some helional for EU/UK, seems to be harder to get than even a year ago.
-
25% yield for this is horrible btw, you could pull a lot more if you didn't cut so many corners.
Can you be more specific? I received over 800 grams of amide from 1000 grams of aldehyde. It's just the final rearrangement where I get low yields so any advice is appreciated.
BTW this synth was the work of a former Hive member named two_dogs. I'm just capitalizing on someone else's work as usual.
-
dont know how i found this thread but glad i did, excellent write up and super snaps!
-
You've got 2 weak spots- the Hoffmann rearrangement and recovering your product.
Knock up a 2.0M hypochlorite solution- 200g NaOH in 1250mL ice water. Set up a chlorine generator (conc HCl dripped onto KMnO4) and slowly bubble Cl2 gas through the NaOH solution until it weighs 140g more than when you started (put the beaker on scales). Adjust the pH with a little NaOH so it's about pH8. (Think the maths is right- will recheck tomorrow, ale-fog)
Use this solution to run the Hoffmann in, start the reaction at 0ºC and allow it to warm to room temperature- expect a bit of an exotherm as you're using much stronger hypochlorite solution than just bleach.
To recover more product, don't try to do a biphasic acidification of the toluene, you lose too much product. Extract a couple of times with toluene (once isn't enough), combine the extracts and dry with Magnesium Sulfate. Filter the MgSO4 off and chill the toluene. Set up an HCl generator (I love my gas generators ;D ) by dripping conc H2SO4 onto NaCl wetted with a little dilute HCl and gas the toluene solution. Filter off the MDA, chill and gas again (you tend to get a couple of crops of product when you gas amine solutions). The MDA should be a lot cleaner and you'll retrieve a lot more product.
Also, I've done some of these Beckmann type rearrangements (the aldoxime to amide step) with different metal salts- in my experience Nickel Acetate works better than NiCl2. Give it a go :D
-
I still can't figure out how to properly read grams on my scale. I doubt I'll be doing this but it's pretty cool though. Never was good in Science classes.
-
Also, it would be good if a vendor could list some helional for EU/UK, seems to be harder to get than even a year ago.
+1
AUS aswell please :)
-
I found it in the US from a perfumery place, 95$ a kg. Is this safe to order under my name? Do you think I will end up on a list or be questioned about my use of it?
-
Nice. I'm always skeptic about the reasons a sellers (by fame a good one) would simply show show the formula of his support. Anyway, if I do something by myself, I would test in a zombie first.
But what about the MDMA pure crystal? ;D ;D ;D ;D ;D ;D ;D
-
You can make MDMA from MDA, not a very efficient route though.
-
You can make MDMA from MDA, not a very efficient route though.
Is there some info on silkroad about the best route to get the so desired pure crystals?
-
I believe there is a writeup in PiHKAL, google is your friend.
-
DO NOT DO THIS OFF EBAY.
I remember reading an article a couple years back about a guy in east coast US who got busted for THIS EXACT SAME THING by LE. He order all his MDxx production tools off eBay, LE noticed somehow, and they caught him mid-batch.
Dont remember exact details, but i can guarantee he is not a free man right now.
-
Knock up a 2.0M hypochlorite solution
I live in a densely populated area so I need to avoid Cl2. What's your thoughts on using calcium hypochlorite instead of sodium? I think I'll give it a go for shits and giggles. Who knows.
-
Yeah calcium hypochlorite should work, with the added advantage of being very OTC.
It'll be pretty exothermic so you may have to run a couple of experiments to determine what works best for you- In one, make a solution of the Ca(OCl)2 first and chill it. In the second, add the Ca(OCl)2 powder directly to the reaction mixture in portions. Have several kg of ice on hand in both cases :P
Averagegatsby- that was the US vs Sicilliano case. Not sure if he was jailed, if I remember correctly a lot of the DEA's evidence was deemed inadmissible. Michael Siciliano doesn't show up on the bop.gov inmate locator.
-
This is incredible thanks DopeBoy. If I remember correctly you're based in Canada, is it easy for someone in the US to acquire these chemicals? And how would you go about ordering/receiving them?
-
This looks really interesting. Do you have any links to sources in chemistry literature or anything like that?
Also, what alternative chems could one use? I know the solvents can be bought at Lowe's I think. Just wondering.
I think the only chem that looks hard to get is the hydroxylamine hydrochloride. Whats the best way one would get this?
Thanks
-
There are heaps of references for the Aldoxime to Amide rearrangement, here's a few
http://pubs.acs.org/doi/abs/10.1021/ja01469a048
http://www.ncbi.nlm.nih.gov/pubmed/20945850
http://onlinelibrary.wiley.com/doi/10.1002/adsc.201100650/full
The other 2 reactions are trivial (the aldoxime formation and Hoffmann).
If you can't find a place to buy hydroxylamine, you can make it by refluxing nitromethane, HCl and water. It's not a reaction I'd be enthusiastic about running, not least as you'd have to distill lots of nitromethane. There's a nice prep here:
http://www.sciencemadness.org/member_publications/energetic_glyoxime_and_diaminofurazan_derivatives.pdf
but the yields are shitty. The second prep is better, I can't imagine a better way of alerting the authorities to your activities than heating a sealed tube containing a liter of nitromethane to near boiling :-\
-
Averagegatsby- that was the US vs Sicilliano case. Not sure if he was jailed, if I remember correctly a lot of the DEA's evidence was deemed inadmissible. Michael Siciliano doesn't show up on the bop.gov inmate locator.
Fair enough, thanks for clarifying wowz.
He may not be incarcerated, but it does prove LE knows about this. Just my .02
-
If I remember correctly you're based in Canada, is it easy for someone in the US to acquire these chemicals?
Yes. And it's getting easier every year. The more we go out and spend money on lab equipment and chemicals, the more chemical companies will flourish and grow to meet our demand. And when US companies fail to meet the demand, Chinese and Indian companies will fill the void.
Google these words - canada scientific glassware - and there should be at least a dozen good suppliers within the first 5 pages. Who cares if they're friendly or not... they either accept your money or not. And if not go to the next supplier lol. We're not begging them to take our money, they should be happy to get your business that's the way business is supposed to work. Yes many North American businesses have gotten spoiled and some of them will turn their noses up at us. It's to be expected. Just brush it off and remember that there's 80 million Chinee currently still making a dollar a day who will cater to our every need.
-
Thanks for posting this. I remember being impressed with first hearing it years ago. I love the pics and the way you have broken it down. Now..at the risk of sounding to dumb to ever complete this synth....could you tell me what you mean by substrate in the first step?
-
most of these do not need to be bought online
* alpha-methyl-3,4-(methylenedioxy)hydrocinnamaldehyde [CAS#1205-17-0]-can be purchased at from perfume companies as ocean propanol or chem supply companies as helional.
* hydroxylamine hydrochloride-can be purchased online
* nickel acetate-can't find any in person shop that sells this atm however you can get it for your nickel plating experiments. Although it is not that hard to synth.
* methanol-look for "heet fuel line antifreeze" at an auto shop
*[or ethanol can be used]-home depot, look for "denatured alcohol"
* sodium carbonate-check a supermarket in the cleaning section, or a pool store as water softener
* sodium hydroxide-drain cleaner, the stuff in stores is typically not very usable for lab purposes. look for the type used in soap making
* household bleach-if you have trouble here then go die
* xylene-also home depot another type of paint thinner
* hydrochloric acid-home depot look for "muriatic acid"
* acetone-also home depot "paint thinner"
-
most of these do not need to be bought online
* alpha-methyl-3,4-(methylenedioxy)hydrocinnamaldehyde [CAS#1205-17-0]-can be purchased at from perfume companies as ocean propanol or chem supply companies as helional.
* hydroxylamine hydrochloride-can be purchased online
* nickel acetate-can't find any in person shop that sells this atm however you can get it for your nickel plating experiments. Although it is not that hard to synth.
* methanol-look for "heet fuel line antifreeze" at an auto shop
*[or ethanol can be used]-home depot, look for "denatured alcohol"
* sodium carbonate-check a supermarket in the cleaning section, or a pool store as water softener
* sodium hydroxide-drain cleaner, the stuff in stores is typically not very usable for lab purposes. look for the type used in soap making
* household bleach-if you have trouble here then go die
* xylene-also home depot another type of paint thinner
* hydrochloric acid-home depot look for "muriatic acid"
* acetone-also home depot "paint thinner"
Most solvents from hardware stores are not anhydrous or contain other solvents mixed in and thus not practical for most lab situations. If you have a fractional distillation setup you can fix that though.
-
Most solvents from hardware stores are not anhydrous or contain other solvents mixed in and thus not practical for most lab situations.
This particular synthesis does not require anhydrous conditions. So hardware store solvents are fine.
Methanol is also called Methyl Hydrate and is usually $10 a gallon.
-
I looked everywhere, but you can´t get alpha-methyl-3,4-(methylenedioxy)hydrocinnamaldehyde easy.
If you sell it on Sr i would buy it!
-
so wait whats the precurser chem?? i dont see it in the list.. maybe i missed it
i thought i was oil of.... clove? cant remember for MDA..
-
helional
-
Ok thanks for the tips with helional!
I ve found some sites which sell it, but there is one problem!
It is illegal in my country or i think Eu.
-
I read that in some helional perpetrates is only 1% alpha-methyl-3,4-(methylenedioxy)hydrocinnamaldehyde.
How many % is in your substrat??
-
Thanks DB!
I'm currently taking elementary organic chem, and I love everything about it!
It's exactly what I imagined chemistry would be like when I was a little kid... all the fun glassware and learning about reaction mechanisms and whatnot
I highly recommend taking an elementary organic chemistry course to anyone looking into getting into this sort of thing.
When I was a kid (17-18) I would read these synth. notes and it was all gobbledegook
Now I actually understand and am confident I could do a pretty good job.
One day, if it all goes south... my mail man will be curious as to why I'm suddenly interested in perfumery :)
EDIT- Could you post your synth route for MDMA? Would be icing on the cake.
-
MDMA
http://www.erowid.org/archive/rhodium/clandestine/gonzo/index.html
http://www.erowid.org/archive/rhodium/chemistry/brightstar.mdma.html
http://www.erowid.org/archive/rhodium/chemistry/mdma.drdrool.html
http://www.erowid.org/archive/rhodium/chemistry/alhg.osmium.html
http://www.erowid.org/archive/rhodium/chemistry/redamin.os-bs.html
-
It's exactly what I imagined chemistry would be like when I was a little kid... all the fun glassware and learning about reaction mechanisms and whatnot
I highly recommend taking an elementary organic chemistry course to anyone looking into getting into this sort of thing.
I know, everytime I buy a new piece of glassware I feel like a kid at christmas. :P My interest though really is only to fight the WOD and by proxy the government.
-
Nice guide.
-
Anybody still have the MDMA refining guide lying around? Used to be one posted to bluelight.ru/OVDB.
I'd rather buy cheap inferior MDMA and process it to pure crystals than start from scratch and risk importing the precursors.
-
dopeboy is a fucking LEO troll, don't fall for his tricks. stay smart people.
-
Anybody still have the MDMA refining guide lying around? Used to be one posted to bluelight.ru/OVDB.
I'd rather buy cheap inferior MDMA and process it to pure crystals than start from scratch and risk importing the precursors.
You mean an anhydrous acetone wash?
-
quote author=mdmamail link=topic=14484.msg185276#msg185276 date=1334155855]
Anybody still have the MDMA refining guide lying around? Used to be one posted to bluelight.ru/OVDB.
I'd rather buy cheap inferior MDMA and process it to pure crystals than start from scratch and risk importing the precursors.
[/quote]
I did a little tutorial a while back, enjoy...
http://dkn255hz262ypmii.onion/index.php?topic=10767.msg98503
-
This thread is awesome, thanks dope boy. Definitely something I'd consider once i brush up on my chemistry skills.
-
MDMA
http://www.erowid.org/archive/rhodium/clandestine/gonzo/index.html
http://www.erowid.org/archive/rhodium/chemistry/brightstar.mdma.html
http://www.erowid.org/archive/rhodium/chemistry/mdma.drdrool.html
http://www.erowid.org/archive/rhodium/chemistry/alhg.osmium.html
http://www.erowid.org/archive/rhodium/chemistry/redamin.os-bs.html
Check out the Vespiary and the Collective for some serious chemistry discussion. Lot of old Hive members hanging out in those forums. Also Wet Dreams, although much of the discussion there is amongst a bunch of young tweakers arguing the finer points of SnB meth. ::) Still, there is a lot of great info in the WD archives.
-
The collective? Wet dreams?
-
The collective? Wet dreams?
As I understand it, after the Hive went down, some of the members split off and created different forums. The Vespiary and the Collective and Wet Dreams archive appear to share the same, or similar databases. Up to a certain date, the threads and posts are the same in all three forums, then they branch off.
The Vespiary and the Collective have some chemhacks there that could easily work at Merck, Phizer, or Purdue Pharma with the knowledge they possess (or appear to possess as evaluated by my meager standards). Wet Dreams has some pretty smart guys, too, but the forum seems to have been taken over by SnB fanatics, save for a few elder bees trying to guide them to more fruitful pursuits.
I don't have the links handy, as they are saved on another drive, or even know if they should be posted, but they can be found with diligent googling. Their content cannot be accessed without joining the forums, so no actual content is indexed by search engines.
Also of interest... The Zonez and Science Madness. Science Madness is not really an alt/drug/chem board, but there is still serious discussion of of methods and rxns there, just not as they apply to making specific drugs.
-
This thread is awesome, thanks dope boy. Definitely something I'd consider investing time and money into once i brush up on my chemistry skills ;)
It's pretty simple easy shit too. Buying labware/glassware is an investment and basically you can buy essential oils for pennies a gram and turn them into substances that are literally more valuable than gold, gram for gram.
-
I'm sorry to bump a thread so old but i didn't feel that this post needs its own topic. I'm planning on doing this soon and i have everything planned out but i was curious as to were you guys got your helional. i was considering perfumers apprentice but i was curious if there was any out there that is cheaper or maybe even purer
-
Quick question for my chemistry savvy friends here.
If someone sought to take up chemistry as a hobby what sort of essential reading would you recommend he or she start with? I've got no background at all with this stuff but am the type to really throw myself into things like this, would really appreciate a nudge in the right direction.
-
KhanAcademy has a good chemistry and organic chemistry series. You need in-lab experience though to perfect your techniques ;)
-
Everybody at this site should be setting up labs in their homes.
Yeah coz a bunch amateurs fucking around trying to make designer drug, who will end up with god knows what and then poison a bunch of innocent people. Solid idea genius.
Trust me if an ADHD learning impaired dummy like me can do it, ANYONE can.
-
Marceline, thanks so much!
-
You need in-lab experience though to perfect your techniques ;)
Yup practice makes perfect.
-
does anyone know if cinnamaldehyde will work for this? i've been looking for an answer all day but can't find one. i ask because cinnamaldahyde is found naturally occuring in cinnamon from the grocery store
-
does anyone know if cinnamaldehyde will work for this? i've been looking for an answer all day but can't find one. i ask because cinnamaldahyde is found naturally occuring in cinnamon from the grocery store
You'd need to get the 3,4-methylenedioxy group on there somehow first, which would give you helional. Probably easier to just buy helional from China.
-
would china be the best supply source? or should i go domestic. Is helional even watched? i can't find any evidence saying it is
-
would china be the best supply source? or should i go domestic. Is helional even watched? i can't find any evidence saying it is
Domestic companies are guaranteed to cooperate with cops. Best bet is China.
-
first u.s person to start making mda bulk pm me i might have access to press
-
Quite interested in trying this, my buddys dad owns a chemistry company and he said I could barrow some equipment if I needed so I have some reduced start up costs. Before I buy bulk I would like to try make a small amount to see if I can actually do it. Can any one suggest a site that sells small amounts of the listed chems most important Helional I dont want to invest in a $1000 killo just to find out I can't do it.
-
Would it be possible that some governments have also fucked up Heli by putting some strange molecules in it like commercial mdp2p?
-
Would it be possible that some governments have also fucked up Heli by putting some strange molecules in it like commercial mdp2p?
No.
Here's some picks of the Hoffman reaction.
http://xfq5l5p4g3eyrct7.onion/upload/9100de45284045a231d34f5cbfadf38c.jpg
http://xfq5l5p4g3eyrct7.onion/upload/941ada0406f8ce16e901c9d5bd78db66.jpg
http://xfq5l5p4g3eyrct7.onion/upload/23a32dc9e8eded2d7bdfb43b0f5937f9.jpg
http://xfq5l5p4g3eyrct7.onion/upload/a6d4941669b68077c57ce7e8b8c467d2.jpg
http://xfq5l5p4g3eyrct7.onion/upload/0ccb482127338efcdd63fb82acbe28c9.jpg
http://xfq5l5p4g3eyrct7.onion/upload/cb18994ce03ab17c4d48175db4461167.jpg
http://xfq5l5p4g3eyrct7.onion/upload/04c1d925570d7695318fabc5e205438c.jpg
http://xfq5l5p4g3eyrct7.onion/upload/373355c611b0438ace15557548f40d54.jpg
http://xfq5l5p4g3eyrct7.onion/upload/58f099da22b93251bf2c5758c0ff5422.jpg
http://xfq5l5p4g3eyrct7.onion/upload/b8e470404335b2e4144bb97df24306ad.jpg
http://xfq5l5p4g3eyrct7.onion/upload/1cc9a24a5673125418687c8187559199.jpg
http://xfq5l5p4g3eyrct7.onion/upload/b4c2c8374998c484d8e8bc45c251f41d.jpg
http://xfq5l5p4g3eyrct7.onion/upload/ac9c211346814bd8d4fda27ab2e6bc5d.jpg
http://xfq5l5p4g3eyrct7.onion/upload/81cdcbbe1a77545f0f5000af3494aae6.jpg
http://xfq5l5p4g3eyrct7.onion/upload/8b9b661b8230073fcde79dd7ea7f5d6f.jpg
http://xfq5l5p4g3eyrct7.onion/upload/b7501ecb29c7edb2f00397d09e6b00f9.jpg
http://xfq5l5p4g3eyrct7.onion/upload/edb1aa54945fd633c6cd309f8cc0bfa6.jpg
http://xfq5l5p4g3eyrct7.onion/upload/6f7e01d1a759b778cc313e9a0cf10281.jpg
http://xfq5l5p4g3eyrct7.onion/upload/35eb2b97d4d192202166262841cc8997.jpg
http://xfq5l5p4g3eyrct7.onion/upload/4d6de628a48ec7e52f08a145827538d2.jpg
http://xfq5l5p4g3eyrct7.onion/upload/5e9488429c4b668155f48d4c1186773f.jpg
-
http://img267.imageshack.us/img267/7972/52270169.jpg
http://img191.imageshack.us/img191/34/82086418.jpg
http://img713.imageshack.us/img713/1192/99026897.jpg
http://img96.imageshack.us/img96/3998/44445470.jpg
http://img4.imageshack.us/img4/2056/33931074.jpg
http://img94.imageshack.us/img94/8577/88900480.jpg
http://img811.imageshack.us/img811/6919/21970114.jpg
http://img819.imageshack.us/img819/7964/72954742.jpg
http://img69.imageshack.us/img69/7030/43598446.jpg
http://img833.imageshack.us/img833/9062/79613375.jpg
http://img17.imageshack.us/img17/8443/19336278.jpg
http://img402.imageshack.us/img402/189/54032128.jpg
http://img401.imageshack.us/img401/6164/56497884.jpg
http://img594.imageshack.us/img594/7979/53427794.jpg
http://img109.imageshack.us/img109/1061/76114155.jpg
http://img546.imageshack.us/img546/2027/92413507.jpg
http://img267.imageshack.us/img267/9772/37201755.jpg
http://img9.imageshack.us/img9/6126/35575622.jpg
http://img213.imageshack.us/img213/8150/54466816.jpg
http://img141.imageshack.us/img141/7613/36746926.jpg
http://img22.imageshack.us/img22/7417/13043784.jpg
-
Why are you still in stealth dopeboy if all this is going on in the background?
-
Nice to see you drop in dopeboy! I thought you where gone forever, you where the reason I first made MDA and are the reason I sell precursors for it now!
-
Cool thread, did you know most of the things you need to synth LSD are on ebay?
You guys need to check out my products link.
Dopeboy hit me up if you are interested in some tips for your hoffman
-
btw any advice for someone who messes up the ALDEHYDE --> OXIME step almost 50% of the time, I can never get it to solidify could my problem be im using homemade sodium carbonate that still has residual bicarbonate in it? Also what stirring speed should I use?
-
To solidify try washing it in dilute acid solution.
Also use less water during the oximation to feed in the base, this causes problems.
hint hint feed base in dry
-
Thanks :)
I most likely will end up purchasing your guide next time I attempt the synth, im guessing their would be a lot of info not available on the clearnet.
-
So tonight I decided to try the aldehyde to Oxime again. I had a failed reaction that had been sitting in the freezer for about three weeks, Once I pulled it out I poured of the top liquid layer and kept the yellow frozen paste at the bottom, Im not a chemist but I think that the top is just methanol + carbonate which could dilute my second reaction, I then added appropriate amounts of Hydroxylamine hcl+water and methanol. I slowly rotated the glass jar it was in by hand and within 30 minutes, off white/yellow crystals started to appear at the bottom. I am guessing the reason it worked so well this time was less carbonate, I have read forum chatter that suggested to much sodium carbonate can stop it from solidifying.
I'll up date later with more pics and info on how the other steps go.
http://4eiruntyxxbgfv7o.onion/imgzapr/upload/P191012_00.56.jpg
Sorry for the low quality pic, the white spots are groups of small crystals stuck together.
-
You've got 2 weak spots- the Hoffmann rearrangement and recovering your product.
Knock up a 2.0M hypochlorite solution- 200g NaOH in 1250mL ice water. Set up a chlorine generator (conc HCl dripped onto KMnO4) and slowly bubble Cl2 gas through the NaOH solution until it weighs 140g more than when you started (put the beaker on scales). Adjust the pH with a little NaOH so it's about pH8. (Think the maths is right- will recheck tomorrow, ale-fog)
Use this solution to run the Hoffmann in, start the reaction at 0ºC and allow it to warm to room temperature- expect a bit of an exotherm as you're using much stronger hypochlorite solution than just bleach.
To recover more product, don't try to do a biphasic acidification of the toluene, you lose too much product. Extract a couple of times with toluene (once isn't enough), combine the extracts and dry with Magnesium Sulfate. Filter the MgSO4 off and chill the toluene. Set up an HCl generator (I love my gas generators ;D ) by dripping conc H2SO4 onto NaCl wetted with a little dilute HCl and gas the toluene solution. Filter off the MDA, chill and gas again (you tend to get a couple of crops of product when you gas amine solutions). The MDA should be a lot cleaner and you'll retrieve a lot more product.
Also, I've done some of these Beckmann type rearrangements (the aldoxime to amide step) with different metal salts- in my experience Nickel Acetate works better than NiCl2. Give it a go :D
+1 for the hypochlorite concentration.
+2 to avoid the biphasic acidifications, bubbling dry hcl through the concentrated DCM/toluene/xyelene extracts will yield a higher purity product before recrystallisation, will save some time with washing (colour impurities etc)
Recrystallisation could be done best from anhydrous acetone I guess.. dry some acetone with MgSO4 or CaCl. Maybe try dual solvent recrystallisation.
Generating HCl gas using sulphuric acid in a flask and dripping 30% HCl solution through it connect drying tube with CaCl2 in there and gas the extracts directly.
-
Hi,
Look into this: http://www.erowid.org/archive/rhodium/chemistry/oxime2amine.zn-af.html
Microwaving the reaction speeds up some stuff ;)
A solution of 350g of NH2OH.HCl in 500ml H2O was added to a solution of 500g 2-methyl-3-(3,4-methylenedioxyphenyl)propanal in 1000ml MeOH while stirring vigorously. 200g Na2CO3 was dissolved in 500ml H2O and cooled in an external ice bath, the cooled solution was added slowly over a 2 hour period, the solution coloured to frothy green and was kept stirring for an additional 12h for precitipation of the oxime. The crystals were filtered and washed thoroughly with water and dried under vacuum.
150g of the dried oxime was added to a solution 3g nickel(II)acetate tetrahydrate and 450ml ethylene glycol, microwaved for 2x 3min at 300w in the microwave. The solvent was removed under vacuum and the product was recrystallised from hot toluene and grinded into dust.
50g of NaOH was added to a solution of 600ml NaOCl in 1000ml H2O and put into a ice bath. 50g of the amide was added and put stirring for 72h. The solution was allowed to stir for 12h in a hot oil bath turning into a milky orange colour, the freebase was extracted with 3x70ml dichloromethane and the extracts were bubbled with dry HCl gas yielding 3,4-methylenedioxyamphetamine as the hydrochloride salt which was then washed with 3x 75ml anhydrous acetone and recrystallized from acetonitrile/2-propanol.
cheers
-
One question, is there a big difference between Floramelon (powder) and Helional (liquid)?
And how much Floramelon is equivalent to 1 kilo of Helional.
-
They have the both molecular weight and they look the same.
Why are they all using the liquid version then?
-
[EDIT: quote removed at request of ihidemuffins]
I have a guide that explains this process that I sell. I can consult.
Helional should be liquid!
-
I have some problems with the amide recrystallization, i haven't dried the amide then put 100g in 100ml of boiling water but every time there is a bit left in the goo.
Do I have to dry the amide before boiling it with water? And would the xylene be clean of amide and just contain left-overs?
-
A lot of times what happens in this process is that the oximation fails, but when it fails a VERY similar compound forms so you think you did it right. Then you do the beckman and the same thing happens. So you end up with an "amide" that is actually something totally different.
test your oxime by putting a matchhead sized chunk on foil and heating it with a lighter, it should snap crackle and pop instead of melting and will leave a very acrid smell in the air.
Are you using perfurmers helional or medical helional?
WTF? I think you would know if you accidentally ordered phenobarbital with the generic name of helional...
"Are you using a liquid or 10,000$ worth of crushed up prescription only pills you accidentally ordered?"
-
subbed
-
Are you using perfurmers helional or medical helional?
WTF? I think you would know if you accidentally ordered phenobarbital with the generic name of helional...
"Are you using a liquid or 10,000$ worth of crushed up prescription only pills you accidentally ordered?"
I say that because on a lot of clearnet sites people post this method and say you can get a kg of helional for 100bucks!! And theyre mostly talking about from perfumers shops. Just throwing it out there.
It is a damn shame! People worked hard and people shouting it out like they are the new shulgin.....
People who don't know there chem don't have to know it.