HRID131388

反应详情

EQUATION

反应方程式

HRID 131388 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Suspend 2-(4,5-difluoro-2-nitro-phenylamino)-thiophene-3-carbonitrile (4.02 g, 14.30 mmol) in ethanol (40.0 ml). Dissolve tin(H) chloride (8.14 g, 42.91 mmol) in 5N HCl (40.0 ml) and then add it to the suspension. Heat the reaction at reflux for 5.5 hours and then cool it to ambient temperature. Cool the mixture for 16 hours in a refrigerator. Collect the resulting precipitate by vacuum filtration and then dry it by pulling a vacuum on it to give 3.53 g (86%) of the title compound as a yellow solid: mass spectrum (ion spray): m/z =252.1 (M+1).

WORKUP

后处理

  1. temperatureHeat
  2. customthe reaction
  3. temperatureat reflux for 5.5 hours
  4. temperatureCool the mixture for 16 hours in a refrigerator
  5. customCollect the resulting precipitate
  6. filtrationby vacuum filtration
  7. customdry it