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Author Topic: Meyer disproportionation reaction  (Read 174 times)

java

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Re: Meyer disproportionation reaction
« Reply #20 on: September 28, 2011, 03:34:57 AM »
Reference Information



Action of Mineral Acids on Primary Nitroparaffins
S. B. Lippincott, H. B. Hass
Ind. Eng. Chem.
1939, 31 (1), pp 118–120
DOI: 10.1021/ie50349a025
¡Prefiero morir de pie que vivir siempre arrodillado!.Emiliano ZapataIt is better to die on your feet than to live on your knees!.......

dingbow

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Re: Meyer disproportionation reaction
« Reply #21 on: September 28, 2011, 03:53:20 AM »
Thanks Java!

Redeemed; yeap, thats the text that made me realise that GAA was not required for the reaction and gave me the idea for the bottle 8)

reDEEMed

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Re: Meyer disproportionation reaction
« Reply #22 on: September 28, 2011, 05:36:10 AM »
Well, this really fucking sucks. Now I have to buy a three neck flask and an additional funnel.

Am I doing a good job acting like this bothers me?

I'll be so happy to finally own those two items, er, I mean damn...

Edit: I really am glad to know where that 'Meyer's' came from. That was irritating me. This is great shit, if I can make a half a kilo of this shit in a day, I have no problem throwing 50 grams at some formaldehyde.
« Last Edit: September 28, 2011, 05:40:18 AM by reDEEMed »
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

hypnos

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Re: Meyer disproportionation reaction
« Reply #23 on: September 28, 2011, 06:59:57 AM »
 I Really like what I'm reading here, aside from those concerns re; Hydroxlamine, however as  the Hcl salt is preffered for this dream, I noticed the, "note of caution though this reaction releases carbon monoxide." as well as formic acid-, which also can be used..to make more CO for Anhydration of some Carboxylic acids...from foxy2...
"    Ahheemmm

      To 200 mL of methanol were added 30 grams of nitromethane and 60 grams of oxalic acid.  The resulting mixture was stirred to form a solution.  The solution was then refluxed at atmospheric pressure at a temperature ranging from 60 to 70C(refluxing), for 20 hours.  Hydroxylamine and formic acid were obtained.

      United States Patent  3,380,807
      Current U.S. Class: 423/387; 562/606 

 How much? E.g. Enough to anhydrate acetic acid, and others? this would bee a handy little addition to in the synth process...Make your own anhydrous acids using the excess ( and vented/wasted ) CO...

 BTW; what does one "call" a substance that does an-hydrate carboxylic acids? IS there one, I doubt its a "dessicant" coz its a molecular reaction, CO2 => CO by stripping one of Dioxygen's oxygen atoms....?....anybody?

 Cheers hyppy,
                         btw, lugh, that is an amazing amount of datum you have provided! thanx a lot!!!
 
« Last Edit: September 28, 2011, 07:26:42 AM by hypnos »
"the two things you can give away and never lose, are what you know, and how you feel...."

reDEEMed

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Re: Meyer disproportionation reaction
« Reply #24 on: September 28, 2011, 07:23:25 AM »
For hypnos

hxxp://www.shroomery.org/forums/showflat.php/Number/9390283#9390283

lol
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

hypnos

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Re: Meyer disproportionation reaction
« Reply #25 on: September 28, 2011, 07:47:29 AM »
 Bro, no offence meant, but, surely you would Know, that I am NOT trying to "fractionally distill" AA from GAA
definitely a LOL and IF I WERE that "ignorant" I wouldnt be spending the time I DO here, and other places.... ::)

 That said, one of my EARLIEST posts here, which was given a  Beautiful answer, with Pics and All, was about making anhydrous acids via bubbling various gases through an acid, to obtain the ANhydrous form of the relevant acid 8) 8) 8)

 But you are moving along much faster than I at the moment, sadly for me :'(

 Btw. arent you just a little scared/fearful, "somebody" maybe  'accidentally' bump that beautiful setup?   I'm SURE you must know of 'retort stands',  no? :o

 Peace love and Progress in The Dreams ;D

Hypnos 8)
"the two things you can give away and never lose, are what you know, and how you feel...."

reDEEMed

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Re: Meyer disproportionation reaction
« Reply #26 on: September 28, 2011, 09:07:04 AM »
I was teasing. I don't think anybody would willfully do any of that shit. The last line of that post is really what is relevant, just buy the shit.

Edit: For the fist time I'm nervous handling this stuff. My 90mm Buchner is full to the brim with freebase and it's dry at this point drying out. I'm trying to find solubility data so I can make a strong solution and just keep that on hand in addition to a salt or two. While googling for such info I came across this. I just thought I'd include it because everybody seems so unclear about exactly when and even if the freebase is explosive. Evidently the people who wrote this document are just as confused, but it's more info and more info never hurts.

Post edit edit: Now that I'm specifically googling freebase and ways to make a stable solution, I'm getting lots of documentation on the explosion risk. It seems to me that they are basing all this on a single accident and even there it's unclear exactly what caused it. What we need is a brave soul to produce 800lbs of the freebase in their home to replicate these results, maybe then when can identify the trigger. Hypnos, how about you? You down for helping the community?

Storage and Use of Hydroxylamine Free Base (NH2OH)
Quote
Lesson Learned Statement
Very pure 50 wt% hydroxylamine stabilized solutions are considered safe. However,
extensive stabilizer additives are vital to their safe storage. Safe handling and storage of
these solutions are also affected by contamination with metal ions, excessive
temperatures above 35C, inadvertent concentration, and containment. At greater
concentrations than 50 wt%, hydroxylamine solutions can be potentially hazardous.
« Last Edit: September 28, 2011, 12:32:10 PM by reDEEMed »
"Ego is a structure that is erected by a neurotic individual who is a member of a neurotic culture against the facts of the matter. And culture, which we put on like an overcoat, is the collectivized consensus about what sort of neurotic behaviors are acceptable."
— Terence McKenna

hypnos

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Re: Meyer disproportionation reaction
« Reply #27 on: September 28, 2011, 01:50:49 PM »
"It seems to me that they are basing all this on a single accident and even there it's unclear exactly what caused it. What we need is a brave soul to produce 800lbs of the freebase in their home to replicate these results, maybe then when can identify the trigger. Hypnos, how about you? You down for helping the community?" 

LMFAO!!! thanx steely, I can rely on you for "good Ideas" 8) 8)

 Matey 50ml is "scaling up!" for me!!! in my current state of incapacity,,and hey, wasnt it me that first 'voiced concerns" (at least on this forum...) about "unknown     reasons"for factories (i found of 2 in the past decade!!) which Self Detonated, EVEN WHEN, THERE ARE SUPPOSEDLY TRAINED INDUSTRIAL CHEMISTS running the show.. :o ???
 
lugh has posted a Wealth of information on this subject, in the Hydroxlamine thread..(Including ideas of all sorts, check it out!)
   ..in which these 'concerns' are not ONLY Well covered (12 years AGO!!!) ??? 8)

      and only thanx to lugh would I have found them, AFTER reading/researching for few More Years !!!)
    But as I said, even grinding DRY Hydroxylamine HCl is a bit of a "you go first" activity!! as far as I'm concerned, however there will most probably be some almost 'microscale' in size Dreams on the whiteboard/garage floor/bench  ;) :P

 Thanx for a good laugh, man of Steel

 Ur grateful fellow Vesparian ;D ;)

 Hypnos 8)
"the two things you can give away and never lose, are what you know, and how you feel...."
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