Organic Syntheses, Coll. Vol. 2, p.139 (1943); Vol. 17, p.43 (1937).
solution is separated and washed twice with 100 cc. of water, once with 200 cc. of 5 per cent potassium hydroxide
, and twice with water. If the solution is not colorless it is clarified with 1 g. of Norite
. The benzene
is removed by distillation, and the resulting syrup is dissolved in 300 cc. of alcohol
by heating. The solution on cooling deposits cholestanone
as well-formed needles. The yield of collected, washed, and air-dried material, m.p. 129–130°
, is 41.5–42 g.
per cent of the theoretical amount). The addition of 80 cc. of water to the filtrate gives about 2 g.
of material melting at 125–126°
Material melting at 140–141° (p. 191)
is satisfactory. The presence of a trace of cholesterol
is not objectionable since this is converted into acidic products which are removed in the course of the purification.
When the solutions are mixed without cooling the temperature rises to about 60° and the yield is somewhat less.
The checkers employed a Hershberg stirrer (p. 117)
The agitation may be continued twice as long without appreciable difference in yield. Six hours is regarded as the minimum time for the quantity specified.
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