Organic Syntheses, Coll. Vol. 2, p.5 (1943); Vol. 10, p.1 (1930).
Then 410 g. (251 cc., 3 moles) of bromoacetone (p. 88)
is added, and the mixture is refluxed for sixteen hours on a water bath
at 95–97°. At the end of the operation the solution is cooled to 0° in an ice-salt bath
. The potassium bromide
which settles is filtered on a cooled suction filter
, and the filtrate is fractionated.
The fraction boiling at 23–35°/12 mm. is discarded, as it contains very little acetol
. The main fraction distils at 35–47°/12 mm.
and weighs 160 g.
This material is refractionated, and the portion boiling at 40–43°/12 mm.
is collected. The yield is 120–130 g.
per cent of the theoretical amount) (Note 4)
It is necessary to cool the mixture below 50° to prevent loss of the volatile ethyl formate
Technical ethyl formate
was purified by washing with 3 per cent sodium carbonate
solution, then with cold water, drying over anhydrous sodium sulfate
, filtering, and fractionating. Compare p. 180
. It is very important that all the materials used in the synthesis of acetol
be anhydrous, as otherwise condensation products are formed.
If commercial potassium formate
is used it should be dried under reduced pressure at 80°. One and one-half to two moles should be used per mole of the bromo compound.
polymerizes very readily on standing but remains unchanged when dissolved in an equal volume of methyl alcohol
This preparation is referenced from:
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