HRID1090332

反应详情

EQUATION

反应方程式

HRID 1090332 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 36 mg (0.16 mmol) of 1-benzyl-4-ethynyl-3-(1-hydroxyethyl)-2-azetidinone in 2 ml of methylene chloride, 30 mg (0.25 mmol) of 4,4-dimethylaminopyridine and 0.04 ml (0.25 mmol) of benzyloxycarbonyl chloride were added at -10° C. and the mixture was stirred for a night. Ice water was added to the reaction solution and the resultant was extracted three times with methylene chloride. The extract was washed with a saturated solution of NaCl, dried with anhydrous magnesium sulfate, concentrated and purified with 5 g of silica-gel column (hexane:ether 2:3) to give 40 mg of 1-benzyl-3-(1-benzyloxycarbonyloxyethyl)-4-ethynyl-2-azetidinone (yield: 69%).

WORKUP

后处理

  1. extractionthe resultant was extracted three times with methylene chloride
  2. washThe extract was washed with a saturated solution of NaCl
  3. dry with materialdried with anhydrous magnesium sulfate
  4. concentrationconcentrated
  5. custompurified with 5 g of silica-gel column (hexane:ether 2:3)