HRID657954

反应详情

EQUATION

反应方程式

HRID 657954 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

3,N-Dimethoxy-N-methyl-5-trifluoromethylbenzamide (O3.014, 460 mg) was initially charged in THF (15 ml) under at RT Ar dissolved. Thereafter, the mixture was cooled to 0° C., and methylmagnesium bromide (1.5 ml; 3 M in diethyl ether) was added dropwise. Subsequently, the ice bath was removed and the mixture was stirred at RT for 2 h. Then the mixture was admixed with 1 N hydrochloric acid while cooling with ice, diluted with water and extracted three times with EA. The combined EA phases were dried over sodium sulfate, filtered and concentrated. 349 mg of the title compound were isolated.

WORKUP

后处理

  1. dissolutiondissolved
  2. customSubsequently, the ice bath was removed
  3. temperaturewhile cooling with ice
  4. additiondiluted with water
  5. extractionextracted three times with EA
  6. dry with materialThe combined EA phases were dried over sodium sulfate
  7. filtrationfiltered
  8. concentrationconcentrated