HRID659204

反应详情

EQUATION

反应方程式

HRID 659204 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
-10 °C

PROCEDURE

实验过程

A solution of 4-bromo-3,5-dichlorobenzotrifluoride (1 g, 3.4 mmol) in 1.2 mL tetrahydrofurane was slowly added to isopropylmagnesium bromide (15% in THF, 3.3 g, 3.4 mmol) at max. −10° C. After complete addition the reaction mixture was stirred for 30 min at −10° C. Dimethylformamide (0.275 g, 3.7 mmol) was added and the mixture was slowly warmed up. The mixture was quenched with saturated ammonium chloride solution and extracted three times with ethyl acetate. The combined organic phases were dried on sodium sulfate, filtered and evaporated. The crude product was used without any further purification, brown oil (741 mg, 89%).

WORKUP

后处理

  1. custom−10° C
  2. additionAfter complete addition the reaction mixture
  3. temperaturethe mixture was slowly warmed up
  4. customThe mixture was quenched with saturated ammonium chloride solution
  5. extractionextracted three times with ethyl acetate
  6. customThe combined organic phases were dried on sodium sulfate
  7. filtrationfiltered
  8. customevaporated
  9. customThe crude product was used without any further purification, brown oil (741 mg, 89%)