Author Topic: MeNO2 as a MeNH2 substitute? (topic split) (Read 297 times)

Douchermann · « **on:** May 06, 2009, 05:16:49 PM »

Yeah, I was just commenting on what Vesp said.

Hey, V16, you might know this, is there any reason MeNO2 can't be substituted for MeNH2 in the reductive amination of P2P (not substituted). I was arguing with a college chemistry student (what a flaming idiot he was) that claimed the only way people can make... what we're talking about... was with psuedo, and I told him he was wrong. Then when I was explaining the reductive amination, I ran into a brick wall because I never heard of anyone substituting MeNO2 for MeNH2. It's off topic, but so is MeNH2 from hexamine in a formaldehyde aquisition thread

v16 · « **Reply #1 on:** May 06, 2009, 06:13:15 PM »

well if i understand you right your are asking about P2P to MA vs pseudo to MA. I am no MA man, I don't have any first hand experience with it. That said, the Al amalgam reduction should work with either nitromethane or methylamine regardless of the ketone.

But I think you will end up with both D/L isomers with P2P, where as with pseudo you get just D. That might be what your friend is asking about.

Sedit · « **Reply #2 on:** May 06, 2009, 06:46:15 PM »

Substitution does not interfere and has been used extensivly for MDMA synthesis.

Al/Hg reductive amination of MDP2P using nitromethane as methylamine source [Pictures]
http://www.erowid.org/archive/rhodium/chemistry/alhg-meno2.html

Douchermann · « **Reply #3 on:** May 06, 2009, 07:19:40 PM »

Yeah I knew it worked for MDMA, I just wasn't sure if there was some reason why no one reported using it for MA. Either way, thanks

v16 · « **Reply #4 on:** May 06, 2009, 08:55:04 PM »

I think making P2P is a bit daunting for the home chemist. That might be why its not being used.

Sedit · « **Reply #5 on:** May 06, 2009, 09:08:47 PM »

Further off the topic of Formaldehyde
God its a good thing this is a small forum else we would have the users here lost as can be

You really think so V16?

There are so many means to an end I can't see why one would have problems synthesising it from a number of starting materials. If you have BzO then your pretty much home free with the condensation with MEK to MePhBuO if no BzO that can be made from toluene. Theres always BzCl grignards or conversion with KCN to BzCN-->PAA ....

Latly Iv been considering the hydrolysis of Ephedrine to synthesis P2P as it appears that it would aid in the removal from pill material.

Theres just so many paths to follow no one should really find it daunting. If anything its exciting almost like a cat and mouse game because even with my limited Chemistry knowlage there is no way in hell they could ever ban materials I could make it from.

If you wish I could post a mass of ways with ease in a seperate threed. Many of which would work with the methylenedioxy counter parts also.

Douchermann · « **Reply #6 on:** May 06, 2009, 10:15:22 PM »

The MEK condensation is my favorite

. I've never made it all the way to P2P because I was trying to use peroxy acetic acid with H2O2/H2SO4 catalyst instead of the perborate, but I got a runaway with it. I was actually thinking about how well the MEK condensation would work with piperonal and what kind of yeilds could be seen. Hmmm, so what's the rule of this forum, is routes to P2P okay to discuss in the standard topics, but then what you do with the P2P should be kept in the "secret lives of wasps"?

v16 · « **Reply #7 on:** May 06, 2009, 10:21:24 PM »

"
There are so many means to an end I can't see why one would have problems synthesising it from a number of starting materials. If you have BzO then your pretty much home free with the condensation with MEK to MePhBuO if no BzO that can be made from toluene. Theres always BzCl grignards or conversion with KCN to BzCN-->PAA ...."

um, that is beyond the average joe home chemist. We are talking simple chemistry with simple reagents. IME people drawn to MA synthesis are in no way patient enough to try either one of those methods. You ever work with KCN? Not a fun one to make.

Most of them seem to just want to smurf psudeo....

Sedit · « **Reply #8 on:** May 06, 2009, 10:30:04 PM »

benzylhyde+ MEK ----HCL---> MePhBuO + Peracid oxidation ---> P2P ..... no personal experiance yet but its not in anyway out of reach of the home chemist just something that hasn't been destroyed yet due to over use like other means because it looks complicated and names like 2-acetyl-propenylbenzene or Methyl Phenyl Butanone leave begginner running for the door right away.(A good thing in my eyes)

Honestly I dont feel Psudo is easy anymore yet these folks insist on attacking these pills with expensive arsenals of solvents to generate a few grams at a time of goodies. Then scape few thousand matchbooks and huntdown about 20 bottles of iodine all high risk at every step... and for what? By the time your done with material, risk, and time it would be cheaper to go to work and by your dope when you get home.

KCN.... Not pretty but atlest it aint HCN, Dont eat it and be respectful and things can go your way. Not something I would advise though considering alternatives are safer and less work. Same goes for the grignards.

v16 · « **Reply #9 on:** May 06, 2009, 10:44:03 PM »

Isn't benzyldehyde a list I? But that method would work if you had a good amount of benzyldehyde...

Your right though probably easy to find 100g of it that hunt down a few grams of P. You still have to isolate the isomer at the end with P2P, might be another reason it is not used too much.

Sedit · « **Reply #10 on:** May 06, 2009, 10:51:48 PM »

Pick your method there also,
http://www.sciencemadness.org/talk/viewthread.php?tid=2223

There is also assloads of threeds on generation on BzO, your correct there not for the normal meth cook because many wouldn't know what a mol was if it bit them in the ass but for the average few year chem student with a little patiants for multi step synthesis a quarter pound finish is not out of the question with a week or two work. LOL how much does a quarter pound of MA go for nowdays... alot more then any paycheck Iv ever gotten.

... Low overhead also.

Iv heard claims of L-isomers helping in the protection of neuro damage in MA use also so I dont see much point in resolution steps because for me the shit is to strong anyway and half potancy wouldn't phase me a bit.

Vesp · « **Reply #11 on:** May 06, 2009, 11:47:25 PM »

Haha we should try to work on staying on topic sometime. Does it bug any members?

That one place is just for posting things you don't want others to see. If you don't care, you can post it in the drug synthesis section.

Sedit · « **Reply #12 on:** May 07, 2009, 01:15:49 AM »

Yeh we never have been very good at that have we

Can ya split it where Douchermann asked about the NitroMethane?

Douchermann · « **Reply #13 on:** May 28, 2009, 04:39:54 PM »

Hmmm, I've got a new question about MeNO2 vs MeNH2. I've recently done a reductive amination using MeNH2*HCl and I obtained very high yeilds ~94%. Upon reading about people attempting the MeNO2 method, I've found that their yields are no where near this great (commonly see 18g of product from 25g of ketone, which is about a 56% yeild). Is this a because of an inherent flaw of the method? or are these yields just piss poor because of operator mistakes.

Sedit · « **Reply #14 on:** May 28, 2009, 06:20:27 PM »

More then likely a little bit of both. The MeNO2 methods have 10% lower yeilds stated by Bio over at the zones. This is one of the reasons that many people advocate making your MeNH2 the correct way and using that instead. Using MeNO2 the MeNH2 has to be generated and used right away and since the heat is so high you can expect some loses in the process. Maybe this could be over come by excess but that is unclear at the moment.

v16 · « **Reply #15 on:** May 29, 2009, 02:54:28 AM »

there is alot of talk recently about trying to boost nitromethane based reduction yields. Alot of ideas are floating about, but I think a 10% less yield when done right sounds about spot on. One thing I think alot of people miss is using ice cold or even glycol w/dry ice to circulate in their condenser. I think alot of methylamine goes right out the stack.

I think this is why the common argument is to get all the nitromethane in as fast a possible, it gets the reaction over as quick as possible.

Also, when methylamine is used you tend to use a huge excess. This helps to drive the reaction to completion. Kind of hard to do with nitromethane. Moreover the excess methylamine acts to draw up excess h20.

Which one to use really is a personal choice based on your own situation. Some people don't want kg's of methylamine sitting around. Also if you have a good supple of precursors, yield is not that big of a deal. If you busted your ass steam distilling plant matter, I would want to get every last drop one could make.

time2poop · « **Reply #16 on:** June 03, 2009, 08:04:49 PM »

Quote from: v16 on May 29, 2009, 02:54:28 AM

there is alot of talk recently about trying to boost nitromethane based reduction yields. Alot of ideas are floating about, but I think a 10% less yield when done right sounds about spot on. One thing I think alot of people miss is using ice cold or even glycol w/dry ice to circulate in their condenser. I think alot of methylamine goes right out the stack.

I think this is why the common argument is to get all the nitromethane in as fast a possible, it gets the reaction over as quick as possible.

Also, when methylamine is used you tend to use a huge excess. This helps to drive the reaction to completion. Kind of hard to do with nitromethane. Moreover the excess methylamine acts to draw up excess h20.

Which one to use really is a personal choice based on your own situation. Some people don't want kg's of methylamine sitting around. Also if you have a good supple of precursors, yield is not that big of a deal. If you busted your ass steam distilling plant matter, I would want to get every last drop one could make.

wouldn't dropping in the nitro first and producing the methylamine first actually give it more time to possibly escape through the condenser instead of dropping the ketone/nitro in together and let the imine and methylamine react as quickly as possible. i guess what i'm thinking is that the longer the methylamine is waiting for the imine, the better chance of it escaping through the condenser? whether or not methylamine is soluble in the MeOH used, its boiling point is -6C so it would boil right out of the MeOH wouldn't it? that would make one think its better to drop it all in at once because you can't get a condenser cold enough to condense the methylamine using just water (the average joe).

v16 · « **Reply #17 on:** June 03, 2009, 08:33:19 PM »

dry ice and ethylen glycol will get you there.

Douchermann · « **Reply #18 on:** June 05, 2009, 04:12:23 AM »

actually Abacus from the hive developed a decent method for producing it in two steps. First, dilute (~6%) methylamine solution in methanol is prepared from Al/Hg on nitro, this is distilled and used as the solvent and methylamine source in the reductive amination. Once I get it to work, I will post the method. My problem right now is the nitro reduction is terminating about 25% of the way through. I'm going to try with aluminum foil instead of thick foil, then I'll try refluxing overnight. My titrations typically gave me about a 1.5% methylamine solution after distillation. Not a whole lot of methylamine escapes if it's dilute.

ChesireCat · « **Reply #19 on:** August 14, 2009, 07:19:26 PM »

Quote from: v16 on May 06, 2009, 06:13:15 PM

well if i understand you right your are asking about P2P to MA vs pseudo to MA. I am no MA man, I don't have any first hand experience with it. That said, the Al amalgam reduction should work with either nitromethane or methylamine regardless of the ketone.

But I think you will end up with both D/L isomers with P2P, where as with pseudo you get just D. That might be what your friend is asking about.

V16 is absolutely correct. MeNO2 Or MeNH2 makes no difference the result is the same.

CC

Author Topic: MeNO2 as a MeNH2 substitute? (topic split) (Read 297 times)

Douchermann

MeNO2 as a MeNH2 substitute? (topic split)

v16

MeNO2 as a MeNH2 substitute? (topic split)

Sedit

MeNO2 as a MeNH2 substitute? (topic split)

Douchermann

MeNO2 as a MeNH2 substitute? (topic split)

v16

MeNO2 as a MeNH2 substitute? (topic split)

Sedit

MeNO2 as a MeNH2 substitute? (topic split)

Douchermann

MeNO2 as a MeNH2 substitute? (topic split)

v16

MeNO2 as a MeNH2 substitute? (topic split)

Sedit

MeNO2 as a MeNH2 substitute? (topic split)

v16

MeNO2 as a MeNH2 substitute? (topic split)

Sedit

MeNO2 as a MeNH2 substitute? (topic split)

Vesp

MeNO2 as a MeNH2 substitute? (topic split)

Sedit

MeNO2 as a MeNH2 substitute? (topic split)

Douchermann

Re: MeNO2 as a MeNH2 substitute? (topic split)

Sedit

Re: MeNO2 as a MeNH2 substitute? (topic split)

v16

Re: MeNO2 as a MeNH2 substitute? (topic split)

time2poop

Re: MeNO2 as a MeNH2 substitute? (topic split)

v16

Re: MeNO2 as a MeNH2 substitute? (topic split)

Douchermann

Re: MeNO2 as a MeNH2 substitute? (topic split)

ChesireCat

Re: MeNO2 as a MeNH2 substitute? (topic split)