HRID74483

反应详情

EQUATION

反应方程式

HRID 74483 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
100 °C

PROCEDURE

实验过程

A mixture solution of 5-iodo-2-methyl-1H-benzimidazole (10 g, 39 mmol), trimethoxy-methane (200 ml), and chlorotrimethylsilane (0.075 ml, 0.59 mmol) was heated and stirred at 100° C. for five hours under a nitrogen atmosphere while distilling off the solvent (a reaction conversion rate of 97%). The reaction mixture was cooled to 40° C., and then a tetrahydrofuran solution (0.87 ml, 0.87 mmol) of potassium tert-butoxide was added thereto. This was concentrated under reduced pressure to provide crude 1-dimethoxymethyl-5-iodo-2-methyl-1H-benzimidazole.

WORKUP

后处理

  1. distillationwhile distilling off the solvent (a reaction conversion rate of 97%)
  2. temperatureThe reaction mixture was cooled to 40° C.
  3. concentrationThis was concentrated under reduced pressure