HRID912250
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
To a DMF solution (15 ml) of N-(3-bromo-phenyl)-acetamide (1.19 g) obtained in Step A, 60% oily sodium hydride (279 mg) was added, followed by stirring at room temperature for 10 minutes. To this, methyl iodide (434 μl) was added, followed by stirring at room temperature for 21 hours. To this, water (30 ml) was added, followed by extraction with ethyl acetate (30 ml×2), and the organic layer was dried over sodium sulfate. The sodium sulfate was filtered off, followed by purification by silica gel column chromatography (dichloromethane/methanol=200/1), to obtain the desired compound (1.20 g, 94%).
WORKUP
后处理
- stirringby stirring at room temperature for 21 hours
- extractionfollowed by extraction with ethyl acetate (30 ml×2)
- dry with materialthe organic layer was dried over sodium sulfate
- filtrationThe sodium sulfate was filtered off
- customfollowed by purification by silica gel column chromatography (dichloromethane/methanol=200/1)