HRID1421557

反应详情

EQUATION

反应方程式

HRID 1421557 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 11.2 g. of 7a-propyl-3-O-methylestrone 5 in 60 ml of toluene were added 6 ml of dimethylhydrazine and 0.5 ml. of trifluoroacetic acid. The mixture was refluxed for 1.5 hr. After cooling to r.t. the reaction mixture was neutralized with 5% NaHCO3 and the organic layer was washed several times with water and dried over sodium sulfate. After concentration and chromatography 11.4 g of the hydrazone 6 remained as an oil; Rf 030 (hept/ethylac. 7/3).

WORKUP

后处理

  1. temperatureThe mixture was refluxed for 1.5 hr
  2. washthe organic layer was washed several times with water
  3. dry with materialdried over sodium sulfate
  4. concentrationAfter concentration and chromatography 11.4 g of the hydrazone 6