HRID971520

反应详情

EQUATION

反应方程式

HRID 971520 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 p-nitrobenzyl α-[4-cyclopropylmethoxycarbonylthio-3-phenoxyacetamido-2-oxoazetidin-1-yl]-α-(2-bromo-1-hydroxyethylidene)acetate (281 mg) in methanol free methylene chloride (2.1 ml) is added aluminum chloride (220 mg) under ice cooling, and the mixture is stirred under argon atmosphere. After 35 minutes, the reaction mixture is poured into ice water containing 4N-hydrochloric acid (4 ml). stirred for 10 minutes, and is extracted with chloroform. The extract solution is washed with water, dried and evaporated to give p-nitrobenzyl α-[4-mercapto-3-phenoxyacetamido-2-oxoazetidin-1-yl]-α-(2-bromo-1-hydroxyethylidene)acetate (150 mg). Yellow foam. Yield: 94.6%. IR: vmaxCDCl3 3400, 1780, 1692, 1610, 1603 cm-1. NMR: δCDCl3 2.25d(10Hz)1H, 4.25d(2Hz), 4.58s2H, 5.20-5.37m4H, 6.84-8.24m9H, 12.1s1H.

WORKUP

后处理

  1. stirringstirred for 10 minutes
  2. extractionis extracted with chloroform
  3. washThe extract solution is washed with water
  4. customdried
  5. customevaporated