HRID839526

反应详情

EQUATION

反应方程式

HRID 839526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
200 °C

PROCEDURE

实验过程

A mixture of 4.806 g of para-chlorobenzotrifluoride, 0.4991 g of cuprous chloride, 3.103 g of potassium fluoride, 13 g of ammonia, 17.9241 g of methanol, and 0.1961 g of n-undecane was heated at 200° C for 5 hrs in an 80 ml Hastelloy shaker tube. After cooling and venting the ammonia, the product mixture was removed. Most of the methanol and para-chlorobenzotrifluoride were distilled out of the product mixture. The remaining solution was diluted with diethyl ether and extracted with 0.5 M KOH to remove copper and ammonium salts as well as potassium fluoride. The ether layer was dried over CaSO4. Vacuum distillation of the ether layer gave 0.55 g of para-aminobenzotrifluoride.

WORKUP

后处理

  1. temperatureAfter cooling
  2. customthe product mixture was removed
  3. distillationMost of the methanol and para-chlorobenzotrifluoride were distilled out of the product mixture
  4. additionThe remaining solution was diluted with diethyl ether
  5. extractionextracted with 0.5 M KOH
  6. customto remove copper and ammonium salts as well as potassium fluoride
  7. dry with materialThe ether layer was dried over CaSO4
  8. distillationVacuum distillation of the ether layer