2-methylamine synthesis pictorial

Upload: jiskate77

Post on 01-Jun-2018

213 views

Category:

Documents


0 download

TRANSCRIPT

  • 8/9/2019 2-Methylamine Synthesis Pictorial

    1/9

    This fle is a part o the Rhodium site archive. This Aug 2004 static snapshotis hosted by Erowid

    as o ay 200! and is not being updated. " " #ac$ to Rhodium Archive %nde&" "

    ' www.rhodium.ws ( '( ')hemistry Archive(

    ethylamine rom Ammonium )hloride and *ormaldehyde

    A +hoto,Essay

    -T by Rhodium

    any bees are ma$ing methylamine out o he&amine and -)l acid. % thin$ it/svery time consuming and -)l is pretty nasty. Thus % have ound that one caneasily ma$e lots o good uality methylamine rom ammonium chloride and

    ormaldehyde 1 ormalin . 3nly drawbac$ with this method is that one musthave good uality ormaldehyde. %t may have para ormaldehyde sediment in

    the bottom it doesn/t hurt not even a bit but *ormaldehyde has to be strongand not some diluted shit 5!,406 is fne.

    7ow to the more,less oolproo method. % you do li$e said below you getaround 400,4!0 grams o pretty pure dimethylamine, ree methylaminehydrochloride which is per ect or Al8-g reductive aminations.

    )hemicals needed9

    ::00g o Ammonium )hloride

    2 liters o 5!,406 *ormaldehyde

    about hal a litre o chloro orm

    http://var/www/apps/conversion/tmp/scratch_6/www.rhodium.wshttp://var/www/apps/conversion/tmp/scratch_6/www.rhodium.ws
  • 8/9/2019 2-Methylamine Synthesis Pictorial

    2/9

    The process

    +our your ormaldehyde in a big round bottom ;as$ 1use at

    least one o ! liter capacity along with ammonium chloride

    and stir a bit. % used a :2 R# ;as$. 0=)(

    At about ?0=) an e&othermic reaction $ic$s in 1it needs tobe cooled in a water bath once in a while at the beginning

    in order to $eep temperature below :04,:0@=) .

  • 8/9/2019 2-Methylamine Synthesis Pictorial

    3/9

  • 8/9/2019 2-Methylamine Synthesis Pictorial

    4/9

    eep that temperature 5,4 hours or so then turn heat up and boil water away

    until you see ammonium chloride coming out o solution. )ool to 20=) and

    vacuum flter it oB on large #uchner unnel 1% have one with C 2! cm .

    Dou should get a clear yellowish fltrate li$e in this picture.

  • 8/9/2019 2-Methylamine Synthesis Pictorial

    5/9

    Trans er it to a smaller ;as$ and boil water away until you see

    the internal temperature rise over :@0=) then turn on the vacuum andcontinue

    frst temperature alls a ew tens o degrees and when it rises bac$ to about

    :@0=) the methylamine is almost ree o water. Turn oB the vacuum and theheat.

  • 8/9/2019 2-Methylamine Synthesis Pictorial

    6/9

    +our your crude methylamine hydrochloride in a bea$er. At frst it is still li uid

    1in this picture it has started to solidi y you can still see some orange li uid

    at the bottom o the bea$er .

  • 8/9/2019 2-Methylamine Synthesis Pictorial

    7/9

    hen it has cooled down you/ll have a big chun$ o hard and drymethylamine.

    ash it a ew times with chloro orm and you/ll end up with a ully white mush.

  • 8/9/2019 2-Methylamine Synthesis Pictorial

    8/9

    Facuum flter to get pure and dry ethylamine.-)l which ree$s o chloro orm.

    The smell can be removed by drying in a vacuum desiccator. Go not try touse

    the oven to get rid o these traces o chloro orm the ethylamine.-)l pic$sup

    water rom air li$e nothing. Dou can only use vacuum or sucess ul drying but

    these )-)l5 traces don/t hurt the methylamine at all and may be le t in butyou

    might perhaps be a per ectionist...

  • 8/9/2019 2-Methylamine Synthesis Pictorial

    9/9

    *inal yield o snow white non,stic$y powder 1consisting o methylamine witha

    ew percent ammonium chloride but and almost no dimethylamine

    hydrochlorideeasily e&ceeds 400g i everything done correctly or even !00g i you used

    406 ormaldehyde.

    rhodium8chemistry8pictures8space8>&>.gi