HRID703186

反应详情

EQUATION

反应方程式

HRID 703186 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 500 mg of 6-[[(3-methyl-4-nitro-2-pyridyl)methyl]thio]-5H-1,3-dioxolo[4,5-f]benzimidazole in 20 ml of absolute methanol was treated with 300 mg of sodium methylate, whereupon the mixture was boiled at reflux under argon for 18 hours. The reaction mixture was buffered by means of glacial acetic acid and concentrated in vacuo. The residue was treated with methylene chloride/sodium bicarbonate solution, whereupon the organic solution was dried and concentrated. By recrystallization from ethyl acetate there was obtained 6-[[(4-methoxy-3-methyl-2-pyridyl)methyl]thio]-5H-1,3-dioxolo[45-f]benzimidazole of melting point 215°-220°.

WORKUP

后处理

  1. temperatureat reflux under argon for 18 hours
  2. concentrationconcentrated in vacuo
  3. additionThe residue was treated with methylene chloride/sodium bicarbonate solution, whereupon the organic solution
  4. customwas dried
  5. concentrationconcentrated
  6. customBy recrystallization from ethyl acetate