HRID925420

反应详情

EQUATION

反应方程式

HRID 925420 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

i-Propylmagnesium chloride (2 M in THF, 8.98 mL, 17.95 mmol) was added dropwise to a cooled (−30° C.) solution of 4-chloro-1-ethyl-2-iodobenzene (4.35 g, 16.3 mmol) in dry THF (40 mL) and the reaction mixture was stirred at the same temperature for 30 min, under argon. After this time, trimethylborate (3.63 mL, 32.6 mmol) was added dropwise and the reaction mixture was stirred at the same temperature for 1.5 h. HCl (1 M, 16 mL) was added and the reaction mixture extracted with AcOEt (3×50 mL). The combined organic layers were dried over sodium sulfate and, after removal of the solvent, a solid was obtained, which was triturated with hexane to obtain the title compound as a white solid (2.15 g, 72%).

WORKUP

后处理

  1. stirringthe reaction mixture was stirred at the same temperature for 1.5 h
  2. extractionthe reaction mixture extracted with AcOEt (3×50 mL)
  3. dry with materialThe combined organic layers were dried over sodium sulfate
  4. customafter removal of the solvent
  5. customa solid was obtained
  6. customwhich was triturated with hexane