HRID839526
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureAfter cooling
- customthe product mixture was removed
- distillationMost of the methanol and para-chlorobenzotrifluoride were distilled out of the product mixture
- additionThe remaining solution was diluted with diethyl ether
- extractionextracted with 0.5 M KOH
- customto remove copper and ammonium salts as well as potassium fluoride
- dry with materialThe ether layer was dried over CaSO4
- distillationVacuum distillation of the ether layer