反应详情

A solution of 1.0 g (1.5 mmol) of 1α,3β,25-tris[(tetrahydro-2H-pyran-2-yl)oxyl]-cholest-5-en-23-yne in 14 ml of methanol was treated with 50 mg of p-toluenesulphonic acid monohydrate, and the mixture was left at room temperature for 1 hour. 16 ml of water was added dropwise while stirring. The separated material was filtered off under suction and dried. After chromatography on 60 g of silica gel with hexane/ether (1:1) and ethyl acetate, there was obtained 0.49 g (79%) of crystalline 1α,3β,25-trihydroxy-cholest-5-en-23yne of melting point 204°-206° C. Recrystallization of a sample from acetone gave crystals of melting point 205°-206° C.; [α]D25 =-12.6° (c=0.5 in methanol).

1. filtrationThe separated material was filtered off under suction
2. customdried