HRID1983499

反应详情

EQUATION

反应方程式

HRID 1983499 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
-60 °C

PROCEDURE

实验过程

A total of 1.64 ml of diisopropylamine was dissolved in 27 ml of tetrahydrofuran, 6.8 ml of a 1.57 M solution of n-butyllithium in hexane was added at −50° C. under stirring, and the mixture was stirred at −30° C. for 30 minutes. After cooling to −60° C., 2 g of 1-bromo-4-fluoro-2-methoxy-benzene obtained in Production Example II-1-a was added and the mixture was stirred at −60° C. for 1 hour. Then, 1.55 ml of 3-fluoro-benzaldehyde was added, followed by stirring for 1 hour. Saturated aqueous ammonium chloride solution was added to the reaction mixture, and the mixture was extracted with diethyl ether. The resulting organic layer was washed with brine, dried over magnesium sulfate and the solvent was evaporated, to give 2.4 g of the title compound as a yellow-brown oil.

WORKUP

后处理

  1. stirringthe mixture was stirred at −30° C. for 30 minutes
  2. additionwas added
  3. stirringthe mixture was stirred at −60° C. for 1 hour
  4. stirringby stirring for 1 hour
  5. extractionthe mixture was extracted with diethyl ether
  6. washThe resulting organic layer was washed with brine
  7. dry with materialdried over magnesium sulfate
  8. customthe solvent was evaporated