HRID1066847

反应详情

EQUATION

反应方程式

HRID 1066847 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

In a 50 ml flask, under a nitrogen atmosphere, 2-fluoro-5-bromobenzyl alcohol (2.139 g, 10.4 mmol) was dissolved in N,N-dimethylformamide (25 ml). To this solution sodium hydride (60%, 625 mg, 15.6 mmol) was added and the resulting mixture was stirred for twenty minutes. To the reaction mixture 5-chloropentyl bromide was added and the resulting mixture was stirred for two hours at ambient temperature. The progress of the reaction was monitored by thin layer chromatography. Sodium iodide (3.127 g, 20.9 mmol) was added and the resulting mixture was stirred at ambient temperature for three hours. The reaction mixture was diluted with diethyl ether and washed seven times with brine. The solvents were removed in vacuo. The title intermediate was further purified by silica gel.

WORKUP

后处理

  1. stirringthe resulting mixture was stirred for two hours at ambient temperature
  2. stirringthe resulting mixture was stirred at ambient temperature for three hours
  3. washwashed seven times with brine
  4. customThe solvents were removed in vacuo
  5. customThe title intermediate was further purified by silica gel