HRID2079562

反应详情

EQUATION

反应方程式

HRID 2079562 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

300 mg (1.35 mmol) of 3-fluoro-2-methyl-4-trifluoromethylbenzoic acid were initially charged in 5 ml of N,N-dimethylformamide, and 59 mg (purity 60% by weight, 1.49 mmol) of NaH were added. The mixture was stirred for 10 min, and 199 mg (purity 95% by weight, 2.70 mmol) of sodium thiomethoxide were then added. The mixture was stirred at RT for 1.5 h and then heated at 80° C. for 16 h. The reaction mixture was cooled and, for workup, poured into water and extracted with ethyl acetate, and the aqueous phase was then acidified with concentrated HCl. The mixture was extracted twice with t-butyl methyl ether, dried and concentrated. This gave 310 mg of the product.

WORKUP

后处理

  1. stirringThe mixture was stirred at RT for 1.5 h
  2. temperatureThe reaction mixture was cooled and, for workup
  3. extractionextracted with ethyl acetate
  4. extractionThe mixture was extracted twice with t-butyl methyl ether
  5. customdried
  6. concentrationconcentrated