HRID1077221
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Suspend the foregoing dl-3-methoxy-17,17-ethylenedioxy-6-methyl-13-ethylgona-1,3,5(10)-triene (9.0 g) in methanol (200 cc) and concentrated hydrochloric acid (5.0 cc) and heat on the steam bath for 15 minutes. Remove the solvent under vacuum, partition the residue between ether and aqueous sodium bicarbonate and isolate the product. Recrystallize from methanol to obtain the dl-3-methoxy-6-methyl-13-ethylgona-1,3,5(10)-trien-17-one (7.29 g), m.p. 115°-123°C. Recrystallize a small portion to obtain an analytical sample, m.p. 123°-127°C, λ max. EtOH 280 mμ, λ max. KBr 5.75 μ.
WORKUP
后处理
- customRemove the solvent under vacuum
- custompartition the residue between ether and aqueous sodium bicarbonate
- customisolate the product
- customRecrystallize from methanol