反应详情

Compound 5 (117 g) was added dropwise to a stirring suspension of sodium cyanide (37.64 g) in dimethyl sulfoxide (100 ml). The reactor was placed from time to time into an ice bath in order to keep the reaction temperature between 20° C. and 45° C. Addition lasted 60 minutes. The reaction mixture was stirred for another 16 hours, then poured into methylene chloride (500 ml), washed with water (500 ml, then 2×250 ml), and evaporated to dryness. A small sample was purified on a silica gel column, eluting with dichloromethane/hexanes (50:50 v/v).

1. customThe reactor was placed from time to time into an ice bath in order
2. customthe reaction temperature between 20° C. and 45° C
3. additionAddition
4. washwashed with water (500 ml
5. custom2×250 ml), and evaporated to dryness
6. customA small sample was purified on a silica gel column
7. washeluting with dichloromethane/hexanes (50:50 v/v)