HRID1386100

反应详情

EQUATION

反应方程式

HRID 1386100 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
0 °C

PROCEDURE

实验过程

Methyllithium (40 ml, 64 mmol) was added dropwise at 0° C. to a slurry of copper(I)iodide (6.42 g, 33.6 mmol) in diethyl ether (20 ml). After being stirred at 0° C. for 30 minutes, the clear colorless homogeneous cuprate solution was cooled to −78° C. where 3-bromomethyl-1-fluoro-5-methylbenzene (5.15 g, 25.4 mmol) in 10 ml diethyl ether was added. The temperature was allowed to rise slowly. The reaction was quenched at −50° C. with NH4Cl/NH3-buffer (50 ml). Extraction with diethyl ether (3×50 ml), brine (1×100 ml). The organic layer was dried over MgSO4, filtered and the solvents were removed to yield 3.3 g (94%) of the title compound.

WORKUP

后处理

  1. additionwas added
  2. customThe reaction was quenched at −50° C. with NH4Cl/NH3-buffer (50 ml)
  3. extractionExtraction with diethyl ether (3×50 ml), brine (1×100 ml)
  4. dry with materialThe organic layer was dried over MgSO4
  5. filtrationfiltered
  6. customthe solvents were removed