HRID1156045

反应详情

EQUATION

反应方程式

REACTANTS

反应物

HCID79885

tert-Butoxy bis(dimethylamino)methane

C9H22N2O

结构：CC[C@]12CC[C@@H]3c4ccc(OC)cc4CC[C@H]3[C@@H]1CCC2=O

HCID11087833

未命名化合物

PRODUCTS

生成物

结构：CC[C@]12CC[C@@H]3c4ccc(OC)cc4CC[C@H]3[C@@H]1CC(=CN(C)C)C2=O

HCID70545446

未命名化合物

收率 89.5%

AUXILIARIES

试剂、催化剂与溶剂

溶剂HCID702

Ethanol

C2H6O

CONDITIONS

反应条件

温度: 160 °C

PROCEDURE

实验过程

A mixture of 10 g of 3-methoxy-18-methyl-1,3,5(10)-estratrien-17-one and 15 g of bis(dimethylamino)tert.-butoxymethane is stirred for 3 hours at 160° C. After cooling the mixture is combined with 50 ml of ethanol and left at -5° C. for crystallizing purposes. After filtering off and drying, 10.6 g of 16-dimethylaminomethylene-3-methoxy-18-methyl-1,3,5(10)-estratrien-17-one is obtained, m.p. 157°-159° C.

WORKUP

后处理

temperatureAfter cooling the mixture
waitleft at -5° C.
customfor crystallizing purposes
filtrationAfter filtering off
customdrying