HRID35463
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
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
- temperatureat reflux under argon for 18 hours
- concentrationconcentrated in vacuo
- additionThe residue is treated with methylene chloride/sodium bicarbonate solution, whereupon the organic solution
- customis dried
- concentrationconcentrated
- customBy recrystallization from ethyl acetate