HRID912250

反应详情

EQUATION

反应方程式

HRID 912250 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. stirringby stirring at room temperature for 21 hours
  2. extractionfollowed by extraction with ethyl acetate (30 ml×2)
  3. dry with materialthe organic layer was dried over sodium sulfate
  4. filtrationThe sodium sulfate was filtered off
  5. customfollowed by purification by silica gel column chromatography (dichloromethane/methanol=200/1)