HRID131314

反应详情

EQUATION

反应方程式

HRID 131314 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Combine 4-methyl-2-(2-nitro-phenylamino)-benzonitrile (2.46 g, 9.71 mmol), tin(II) chloride dihydrate (6.57 g, 29.71 mmol), 5N HCl (40 ml), and ethanol (40.0 ml). and stir the mixture at reflux. After 8 hours, cool to ambient temperature. Allow the mixture to stand at ambient temperature overnight and chill for an additional 3 hours in the refrigerator. Remove the resulting precipitate by vacuum filtration and dry it under vacuum to give 1.24 g (49%) of the desired compound as a yellow solid: mass spectrum (ion spray): m/z=224.0 (M+1).

WORKUP

后处理

  1. temperatureat reflux
  2. waitAllow the mixture to stand at ambient temperature overnight
  3. temperaturechill for an additional 3 hours in the refrigerator
  4. customRemove the resulting precipitate
  5. filtrationby vacuum filtration
  6. customdry it under vacuum