HRID35463

反应详情

EQUATION

反应方程式

HRID 35463 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 (1.45 mmol) of 6-[[(3-methyl-4-nitro-2-pyridyl)methyl]thio]-5H-1,3-dioxolo[4,5-f]-benzimidazole in 20 ml of abs. methanol is treated with 300 mg of sodium methylate, whereupon the mixture is boiled at reflux under argon for 18 hours. The reaction mixture is buffered by means of glacial acetic acid and concentrated in vacuo. The residue is treated with methylene chloride/sodium bicarbonate solution, whereupon the organic solution is dried and concentrated. By recrystallization from ethyl acetate there is obtained 6-[[(4-methoxy-3-methyl-2-pyridyl)methyl)thio)-5H-1,3-dioxolo[4,5-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 is treated with methylene chloride/sodium bicarbonate solution, whereupon the organic solution
  4. customis dried
  5. concentrationconcentrated
  6. customBy recrystallization from ethyl acetate