HRID1032947

反应详情

EQUATION

反应方程式

HRID 1032947 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

4

PROCEDURE

实验过程

A solution of the compound (1) (1.37 g, 4.26 mmol), 2-(dimethylamino)ethylchloride hydrochloride (1.84 g, 12.3 mmol) and tetrabutylammonium hydrogensulfate (145 mg, 0.43 mmol) in methylene chloride (8.5 ml) and 4N sodium hydroxide (8.5 ml) was stirred under nitrogen atmosphere at room temperature for about 60 hours. The reaction mixture was diluted with water, extracted with methylene chloride, dried over anhydrous magnesium sulfate and evaporated. The residue was purified by column chromatography on silica gel to recover the compound (1) (60% recovery) and to give the title compound (2). Yield 0.45 g (30%).

WORKUP

后处理

  1. extractionextracted with methylene chloride
  2. dry with materialdried over anhydrous magnesium sulfate
  3. customevaporated
  4. customThe residue was purified by column chromatography on silica gel
  5. customto recover the compound (1) (60% recovery)