HRID466330

反应详情

EQUATION

反应方程式

HRID 466330 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A mixture of 81 mg (3.33 mmol) of magnesium and 574 mg (3.75 mmol) of trimethylgermyl chloride was stirred at 40°-50° C. in an atmosphere of argon. To the mixture was added a solution of 729 mg (3.00 mmol) of 2-(3-bromophenyl)-2-methyl-1,3-dioxolane in 10 ml of tetrahydrofuran with stirring. The mixture was refluxed for 2.5 hr. and stirred at room temperature overnight. To the reaction mixture was added petroleum ether and the insoluble substance was filtered off. The filtrate was evaporated to give 874 mg of pale yellow crystals, which were purified by column chromatography on silica gel [eluent: methylene chloride-n-hexane (1:1)] to give 657 mg of white cubes, m.p. 62.5°-63.5° C. (yield 78%).

WORKUP

后处理

  1. stirringwith stirring
  2. temperatureThe mixture was refluxed for 2.5 hr
  3. stirringand stirred at room temperature overnight
  4. filtrationthe insoluble substance was filtered off
  5. customThe filtrate was evaporated