HRID1834802

反应详情

EQUATION

反应方程式

HRID 1834802 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 4-ethylthio-1-(3-methoxycarbonyl-2-thioureido)-2-nitrobenzene (14.0 g), ferrous chloride tetrahydrate (3.04 g), methanol (235 ml) and water (50 ml) was heated to reflux and treated with reduced iron powder (15.5 g) portionwise during 5 minutes. The mixture was heated at reflux with stirring for one hour. Methanol (250 ml) was added and the mixture was again heated to reflux. The hot mixture was filtered and the filtrate was allowed to cool to room temperature. The solid which crystallised on cooling was filtered off to give 2-amino-4-ethylthio-1-(3-methoxycarbonyl-2-thioureido)benzene (7.5 g), m.p. 168° C.

WORKUP

后处理

  1. temperaturewas heated
  2. temperatureto reflux
  3. temperatureThe mixture was heated
  4. temperatureat reflux
  5. temperaturethe mixture was again heated to reflux
  6. filtrationThe hot mixture was filtered
  7. customThe solid which crystallised
  8. temperatureon cooling
  9. filtrationwas filtered off