HRID867858

反应详情

EQUATION

反应方程式

HRID 867858 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

A solution of 1.62 g. tetraethyl methanediphosphonate in 10 ml. anhydrous toluene is added dropwise to 0.2 g. sodium hydride (69%) in 10 ml. anhydrous toluene. After termination of the evolution of hydrogen, 1 g. 4-bromomethyl-1,2,5-thiadiazole in 10 ml. anhydrous toluene is added thereto and the reaction mixture stirred for 12 hours at ambient temperature. A little water is then added and the organic phase is separated off, dried and evaporated. The residue is purified over a column of silica gel (100 g.; elution agent methylene chloride/methanol 98:2 v/v). There is thus obtained 1.18 g. of the desired product in the form of a colourless oil; yield 55% of theory.

WORKUP

后处理

  1. customthe organic phase is separated off
  2. customdried
  3. customevaporated
  4. customThe residue is purified over a column of silica gel (100 g.; elution agent methylene chloride/methanol 98:2 v/v)