Re: Odczynniki-prekursory

Autor: ch. <michalu_at_poczta.fm>
Data: Wed 12 May 2004 - 17:44:41 MET DST
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Ktorz to wie jakie czasy przyjda :)

A jezeli chodzi o chlorowanie acetonu to chyba chlor podstawi sie i z jednej
i z drugirj strony, ta dalej ta kondensacja (a raczej chyba to sie nazywa
postawienie nukleofilowe :) ) to zajdzie z oboma chlorami czyli wyjdzie cos
podoblego ale nie takiego.... Czy nie mowie prawdy ??

Pozdrawiam
Zydor

Chloroaceto otzrymuje sie w wyniku chlorowania acetonu w srodowisku kwasnym
mam podac konkretna reakcje i przepis?
Chloroacetone [1]
Good method of preperation 150 ml acetone 50 ml water 12 g Cupric chloride 6
g lithium chloride. Reflux till reaction completes. Literature states 24
hours but the reaction has a half-life of about 24 minutes at 20°C (same
article half of marker in 24 minutes, the marker being oxygen consumption in
a slightly different reaction), therefore 5 hours is probably sufficient at
reflux.

After reacting, distill everything below 123°C. The still bottoms can be
reprocessed to recover cuprous chloride and lithium chloride. Both can be
recovered by disolving with minimum water. The mix is easily converted to
cupric chloride-lithium chloride by boiling with 20-35% hydrochloric acid.

Redistill slowly through a packed column to remove acetone. This leaves two
fractions one distilling at 89C which is water and chloroacetone and the
second distilling at 121°C which is ?pure? chloroacetone. The second
fraction may contain unsymetrical dichloroacetone I haven't had a sample
analysed. Calcium Chloride will crash the water-chloroacetone mix which
tends to form a colloidal solution.

Chloroacetone must be stabalized with 1% calcium carbonate or 0.1% water if
it is stored or it forms an explosive sludge. Distillation of a
water-chloroacetone mix at 89°C is the most efficient way of separating
unsym-dichloroacetone from commercial products.

Pozdrawiam
Ch
Received on Wed May 12 17:45:44 2004

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