HRID1415064

反应详情

EQUATION

反应方程式

HRID 1415064 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Add 2.0 g. of lithium to a suspension of 2.0 g. of dl-17β-ethoxy-13-ethyl-3-methoxygona-1,3,5(10)-triene, 90 ml. of 1,2-dimethoxyethane, 100 ml. of 1-methoxy-2-propanol, and 300 ml. of ammonia while stirring. Treat with 2.0 g. of ammonium chloride and water, filter off the precipitate and add it to 80 ml. of methanol, 4 ml. of water, and 5 ml. of conc. hydrochloric acid. Stir for one hour and dilute with water. Extract the product with ether and recrystallize it successively from methanol-water and petroleum ether-ether to obtain the title substance, m.p. 95°-97°; ultraviolet peak at 244 mμ (15,900); infrared peak at 6.0 μ.

WORKUP

后处理

  1. additionAdd 2.0 g
  2. additionTreat with 2.0 g
  3. filtrationof ammonium chloride and water, filter off the precipitate
  4. additionadd it to 80 ml
  5. additiondilute with water
  6. extractionExtract the product with ether
  7. customrecrystallize it successively from methanol-water and petroleum ether-ether
  8. customto obtain the title substance, m.p. 95°-97°