n-butylamine condensations

hAzzBEEn · Fri May 13, 2005 6:33 pm

I thought this was good information about the storage of nitropropene crystals.
This is quoted from the "Louis Freeh" Large Scale Methedrine Synthesis from Rhodium's page:

IndoleAmine · Dreamreader Deluxe

True for impure P2NP, not so for very pure bright yellow crystals (mp above 70°C)...

(other substrates polymerize very fast though)

hAzzBEEn · Sat May 14, 2005 12:00 am

IndoleAmine wrote:

IndoleAmine · Dreamreader Deluxe

In my experience P2NP (if recrystallized properly, has to be almost white Wink

) is good for months if kept in a amber glass vessel, tightly sealed and in the fridge....

N-BuNH2 was tried with 3,4,5-trimethoxybenzaldehyde, with good results:

100mmol (19.62g) 3,4,5-trimethoxy-benzaldehyde were placed in a 250ml RBF together with 11ml* nitromethane and 70ml* GAA and mixed until dissolution with good magnetic stirring. Next, 10ml* n-butylamine were added, causing heat evolution and alot of white smoke (butylammonium acetate fumes) while the solution turned a nice yellow. A double-surface condenser and heating mantle were rigged, and the thing was held at slight reflux (gentle bubbling, only occasional dripping from condenser) for 50 minutes and stirred without heating for another 20 minutes. During this time, the solution color progressed from yellow to orange to red to deep reddish-black. The solution was decanted and upon cooling deposited a lot of nice looking, yellow needles, which were filtered at the buchner, washed liberately with d.H2O (the filtrate was saved separately - some more precipitate was observed in it, and will probably be recycled..), and after air drying for a couple hours under a 60W light bulb, the ugly greenish-yellow crystalline mass was recrystallized from boiling MeOH (60ml were used; too much probably) to give nice, plate-shaped yellow/greenish crystals melting definitely above 80°C (proof enough for SWIA that its for sure not the aldehyde anymore.. Wink

), yield 58.5 percent of theory so far (of course there's a bit more to come if the chemist decides to forget about his laziness for one minute.. Very Happy

).

*All volumes were measured at 20°C room temp.

cheers

i_a

methster · Wed Sep 28, 2005 12:08 pm

hi to all users of this great board,

one question is outstanding for me in this topic.
can swim substitute the sec-Butylamine (2-Aminobutane) for n-Butylamine.
n-Butylamine is rarely available. what about methylamine (40% in h2o) ?

thanks in advance

bio · Working Bee

Aldol type condensations eliminate water and give best yields with near anhydrous conditions.

Do a search and you will find info on using MeNH2 which does work.

methster · Thu Sep 29, 2005 1:02 am

thanks bio. i will do some research on it.

i thought you just tell me:
"yes do a substitution (methylamine<->butylamine) in ratio X:Y"

but maybe SWIic will extend his paper and put this information in it.

greetz

icecool · Insistent Chemist

What do you mean methster?

methster · Thu Sep 29, 2005 3:38 am

sorry, i assumed that the cool pdf with p2np/amph was from SWIy.
there is listed n-butylamine. i was missing information that methylamine,ammonium acetate,... also working and how many ml/mol used.

hAzzBEEn · Thu Sep 29, 2005 5:46 pm

Here is a link to one hive thread that refers to this:

benzaldehyde/nitroethane/methylamine condensation

If one would take some time to search through the hive files here, they would find more. SWIh is sure of it. Searching through the files is tedious because the search engine sucks, but one would learn a heap just by finding things he/she isn't looking for. That link was found with the search engine, though. Here is a link to the hive file, in case someone hasn't found them yet:

The Hive: Reviewed

Methster, please don't try to incriminate the members. I'm positive that if icecool posted that amph pdf, he found it stuck to the bottom of his shoe and had nothing to do with what is pictured. AFAIK, members here don't participate in illegal activity.

icecool · Insistent Chemist

Yes the pdf is from SWIIce anyway I think you can find enough on rhodium concerning the ratio's of other catalysts then n-butylamine, like methylamine etc.
Anyway for n-butylamine one uses this ratio:
1 mol benzaldehyde
1,1 mol EtNO2
0,1 mol n-butylamine