Author Topic: Yeee Haaah!! Jon's method DOES TOO work!! Bromosafrole... (Read 2846 times)

Oerlikon · « **Reply #40 on:** January 09, 2011, 11:36:41 PM »

Will buy mol sieve and use it for methylamine but what about NH3!?
Does it form complex with MgSO4!?

Problem is that I live in very humid area and work in basement,so working w/o some reliable
dehydrating agent just wont work,even with expensive p.a. grade IPA I have.

I know that from experience when I used to work a lot with ammonium nitrate!
For example fist full of ammonium nitrate or NaOH become puddle of water in cca. half hour!

You told me that silica gel is no good since bound between NH3 and water is
stronger but than we need to use something that makes complex with water
and isn't effected by IPA and NH3!

There must be something similar thing that doesn't complex with NH3!
CaO,CaCl2...!?

jon · « **Reply #41 on:** January 09, 2011, 11:57:13 PM »

cacl2 complexes ammonia and amines too use mol seives

Oerlikon · « **Reply #42 on:** January 10, 2011, 01:57:07 AM »

But even finest mol sieve catches NH3 as much as water!

I just gone trough some inorganic chemistry scripts and found this info:
ONLY in presence of water NH3 creates small amount of NH4OH,which becomes source
of OH-(aq) and from resulting conditions we get some Mg(OH)2(s) and (NH4)2SO4 (aq)

MgSO4 (aq) + 2NH3 (aq) + 2H2O (l) <-> Mg(OH)2 (s) + (NH4)2SO4 (aq)

If this is true than products are only in traces in conditions we have (fairly dry IPA).
Assuming that some ionic product in IPA/NH3 isn't terrible inhibitor for amination (is it!?)
than there is no reason not to use it.

I can't find any info if MgSO4 catches NH3 as ligand like Cu and some other transition metals.
Only case I know where Mg ion reacts with NH3 is in presence of phosphate.
If you have any info/sources on this,especially on reactivity between alkaline earth metal ions
and NH3 (or aliphatic amines) please give me a link so I can study it.

jon · « **Reply #43 on:** January 10, 2011, 02:17:43 AM »

my point is to use dry methylamine/ammonia from the start a little water gets in there no problem, but if you use aqueous alcohol it won't work.
why fuck with drying agents and all that hassle.
i've used 99% ipa and that worked so it's important to keep it dry but there is a little room for error.

salat · « **Reply #44 on:** January 10, 2011, 02:02:49 PM »

Quote

dry methylamine

There lies the catch - getting dry methylamine without resource to a centrifuge.

Salat

Oerlikon · « **Reply #45 on:** January 10, 2011, 04:50:02 PM »

Centrifuge!?
A gas?!
At home!?
Pardon my ignorance,but only tipe of gas centrigufe I know abbout is one for enriching nuclear material.

Dripping NaOH solution over ammonia or methylamine salt solution will result in very dry gass.
Using some tube filled with CaCl2,MgSO4 etc. in middle of hose will
catch all remaining traces of water.

Your report sounds like 100% sucess,what happened salat!?
Did you get any amine?!

salat · « **Reply #46 on:** January 10, 2011, 08:05:38 PM »

I haven't got that far.

Read the organic synthesis writeup of methylamine to see what I mean by centrifuge.

Salat

Oerlikon · « **Reply #47 on:** January 10, 2011, 08:38:12 PM »

Methylamine.HCl not a gas.
That makes sense!

Any news on other amine,come on,I am waiting!

NeilPatrickHarris · « **Reply #48 on:** January 13, 2011, 03:55:00 AM »

i've been glued to this thread too, good luck!

jon · « **Reply #49 on:** January 19, 2011, 08:48:00 AM »

i've used wet mushy dirty as hell methylamine, you gas it off as cool as possible the oh- ions tell it to go fuck off it does'nt matter how pristine your methylamine is and you know what humid climates i have worked in salat.

salat · « **Reply #50 on:** January 19, 2011, 03:24:09 PM »

Well it takes a bit longer to do things when you're a newb. Formaldehyde wasn't available (the local OTC has excipients in it and it's cheaper to order hexamine). So there was a methylamine cook off to test an old baalchemist/sumarian method. Posted that over at wetdreams.

It's looking like dry IPA is a good solvent for extracting methylamine hcl after the synthesis is finished. Web results indicated Ammonium chloride isn't appreciably soluble in IPA, but going to test that later.

Salat

Oerlikon · « **Reply #51 on:** January 19, 2011, 08:16:40 PM »

Haven't you allready made complete amination to get orange emulsion or something that Jon confirmed it is an amine!? Than is it a boy or what...!?

IMHO,to get excess methylamine after reaction is finished:
After amination is done,put reaction mix in same apparatus you used to create methylamine gas to dissolve in your IPA,
put one tube leading gas to HCl solution and than basify!
All the methylamine gas should dissolve in acid water to get methylamine.HCl,evaporate and use again!
Just be carefull with backflow,and if you don't know how much HCl to use to capture methylamine
give me amount of methylamine rich IPA and halogensafrole you used,I will calculate it for you!

Next time just go with ammonia water solution or ammonium nitrate & NaOH to enrich IPA with NH3(g) and get some MDA.
It's less job than making methylamine...

salat · « **Reply #52 on:** January 19, 2011, 08:24:27 PM »

There really are two people in this household, one of whom has been a hobby chemist since childhood and the other who has about a year experience. So one of us has completed 2 reactions but being sort of a creative and innovative sort tends to do things his own way, so partial success doesn't get reported. The other of us is just doing their first reaction EVER so she tends to get a bit excited about every little success. Especially when its the first go round. Truly great methods are those that newbs can screw up and still get something out of. We are hobby chemists so we are more interested in what we can learn than producing any particular product per se.

I heard ammonia doesn't work very well even for MDA.

Salat

Oerlikon · « **Reply #53 on:** January 19, 2011, 08:56:29 PM »

I know,that is why I try to help you with some advices.
You think that I knew more than you when I stared!? Of course not!
Have some fun and learn in the process,that's the point!
I was just interested if you did anything usefule out of that reaction,
that's all...

NH3 doesn't work well in Al/Hg reductive amination,but it does in this method!
After all,Jon said ti does! That's enough for me!

jon · « **Reply #54 on:** January 19, 2011, 09:21:54 PM »

ammonia works just as well in this reaction, it's simple hard to fuck up if you know what your doing, it's guerilla chemistry.
i got it right the first time around but i got only 30% but still something always better than nothing.

Oerlikon · « **Reply #55 on:** January 19, 2011, 11:15:24 PM »

What did you screwed up first time!? Water?

salat · « **Reply #56 on:** January 19, 2011, 11:47:31 PM »

There was is definitely something there in the first reaction, just still bogged down in the cleanup stage. Ditto for the 2nd but he's handling that one. Takes a few times to get it right.

I'm about at saturation point as far as taking information in. Got a nice hard copy of a vintage Linus Pauling College Chemistry text that is right up my alley as far as readability. I have had college physics and don't quite see what the heck is the difference. Once I get a handle on what is happening at the lower level the rest will fall into place for me. Didn't understand computers until I learned it at the bits and bytes level. That got me through 20 years of changes in the industry before I burnt out on it.

Meanwhile the rest of this is more technique related - reminds me a lot of cooking.

Salat

jon · « **Reply #57 on:** January 20, 2011, 11:03:09 PM »

you know poring over this thread since i have more time now that i converted to islam and stopped jacking it to porn.
i noticed that you worked up you final process you know where you have the methylamine alcohol iodosafrole soup all reacting for some time and observe the color changes.
you added water well that works but i don't like to do that maybe to get a represenative sample but not for the final workup what i do is this:
strip it all off under a aspirator all the methylamine and all of the alcohol down the drain because i don't like me digs smelling of rotten cunt and neither does me neighbors (gotten a few complaints) so all that shit asspirates down the sink and when i can't catch a whiff of alcohol i'm done then i add about an equal volume of water.
usually some goods drop out (a lot of goods and it is'nt that dirty brown mdma it's piss yellow) so if i'm lazy i'll base it to ph 12 and extract with dcm and wash that and evap the dcm then start with the taste ummm!!! and later on the eye wigglin and all that shite.
but if i want to do it right i'll ph it to 3 with some 2N HCl and wash with toulene (mdma salts dissolve in chlorinated hydrocarbons) then base to 12 with some dilute NaOH, extract with dcm then wash with water but i found it really does'nt matter because usually it's a quantitative conversion to amine so there is'nt anything in the first wash anyway.

salat · « **Reply #58 on:** January 23, 2011, 08:52:54 AM »

Still working on it, some days nothing goes right others stuff falls into my lap.

Noticed the earlier remarks about mol sieve. 3A is good stuff - we got about 25 lbs it can be regenerated and is useful for most solvents - don't use it on acetone though - use drierite for that. It takes a little longer using mol sieve so plan ahead but you can get bone dry IPA with it. Usually have to distill it after drying because there's dust from the sieve. It can be dangerous in regeneration - had the oven door in the garage blow open one day while drying some that had MeOH in it. What you do is put the sieve in a flask and dry heat and recover the solvent, then dry it in the oven.

We have a lot of problems with humidity also. We experimented with some methods I dug up on the hive and found that baalchemists/sumarians post regarding extraction of methylamine using IPA works really well. xBee has some nice methylamine crystals growing now.

"methylamine alcohol iodosafrole soup all reacting and observe the color changes"
Can you give me some more details on this because the only color changes I know about are the ones in the creation of the bromo and iodo. I think this is where we're getting screwed up.

Salat

jon · « **Reply #59 on:** January 23, 2011, 11:21:15 PM »

umm did you even react it with methylamine yet?
i thought you did and were working it up i can't tell where your screwing up.
i said before i turns piss yellow rather quickly.

Author Topic: Yeee Haaah!! Jon's method DOES TOO work!! Bromosafrole... (Read 2846 times)

Oerlikon

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jon

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Oerlikon

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jon

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salat

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Oerlikon

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salat

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Oerlikon

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NeilPatrickHarris

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jon

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salat

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Oerlikon

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Oerlikon

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