HRID1075294

反应详情

EQUATION

反应方程式

HRID 1075294 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

The compound of EXAMPLE 2 (7 g) and 100 ml of toluene was stirred and heated to 70°. To this mixture was added, dropwise, a solution of 14 g ammonium dimethyl phosphorodithioate in 200 ml methanol. The resulting mixture was kept at 70° for 6 hours, then the methanol was distilled off. Toluene (400 ml) was added, and the mixture was washed with water, separated, dried and evaporated under reduced pressure. The solid which remained was washed with toluene and filtered. The solid, m.p. 125°-130°, weighed 2.5 g.

WORKUP

后处理

  1. temperatureheated to 70°
  2. additionTo this mixture was added
  3. distillationthe methanol was distilled off
  4. additionToluene (400 ml) was added
  5. washthe mixture was washed with water
  6. customseparated
  7. customdried
  8. customevaporated under reduced pressure
  9. washThe solid which remained was washed with toluene
  10. filtrationfiltered