反应详情

温度

-10 °C

A solution of 5 g. of 16-dimethylaminomethylene-3-methoxy-1,3,5(10)-estratrien-17-one in 150 ml. of toluene is combined dropwise at -10° C. with 28.5 ml. of a 5% solution of methyllithium in ether. After this dropwise addition, the mixture is agitated for 15 minutes at -10° C.; then about 10 ml. of water is gently added in drops, and the reaction solution is poured into about 200 ml. of 0.5 N hydrochloric acid. The organic phase is separated, dried over sodium sulfate, and concentrated under vacuum. After crystallization of the residue from ethyl acetate/ether, 3.9 g. of 16-ethylidene-3-methoxy-1,3,5(10)-estratrien-17-one is obtained, m.p. 139°-140° C.

1. customis combined dropwise at -10° C. with 28.5 ml
2. additionAfter this dropwise addition
3. additionthe reaction solution is poured into about 200 ml
4. customThe organic phase is separated
5. dry with materialdried over sodium sulfate
6. concentrationconcentrated under vacuum
7. customAfter crystallization of the residue from ethyl acetate/ether, 3.9 g