HRID868322

反应详情

EQUATION

反应方程式

HRID 868322 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Heat a mixture of 466 g (3.72 moles) of 2-aminothiophenol, 250 g (1.24 moles) of 2-chloro4-nitrobenzoic acid, 1.25 liters of quinoline, 192 g (1.34 moles) of cuprous oxide and 125 ml of pyridine in an oil bath at 160°-170° C. with mechanical stirring for 90 minutes. Cool the mixture to room temperature and add 1.87 liters of concentrated hydrochloric acid followed by 625 ml of water. Separate the precipitate and wash well with water. Extract the washed precipitate into boiling methanol and filter. Treat the hot filtrate with charcoal, filter and strip to dryness. Dissolve the residue in aqueous sodium hydroxide, filter and treat with charcoal. Acidify the filtrate and separate the precipitate. (Yield: 38 g).

WORKUP

后处理

  1. temperatureHeat
  2. customSeparate the precipitate
  3. washwash well with water
  4. extractionExtract the washed precipitate
  5. filtrationfilter
  6. additionTreat the hot filtrate with charcoal
  7. filtrationfilter
  8. dissolutionDissolve the residue in aqueous sodium hydroxide
  9. filtrationfilter
  10. additiontreat with charcoal
  11. customseparate the precipitate