HRID1980526

反应详情

EQUATION

反应方程式

HRID 1980526 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 10.0 g (30.6 mmol) of chloromethyl[bis(4-fluorophenyl)](2-propoxy)silane and 3.1 g (30.6 mmol) of 1,2,4-triazole sodium salt in dimethylformamide was stirred at 80°-90° under nitrogen for 2 hours. Workup as in Example 37 gave a waxy solid that was washed with 1:1 ether-hexanes to leave 3.0 g (30%) of the title compound. Recrystallization from chlorobutane gave a purer sample: m.p. 130°-131°; nmr (CDCl3) 4.1 (2H, s), 5.8 (1H, broad s), 7.1 (4H, t), 7.7 (4H, d of d), 7.8 (1H, s), 8.0 (1H, s).

WORKUP

后处理

  1. customWorkup as in Example 37 gave a waxy solid
  2. washthat was washed with 1:1 ether-hexanes