HRID1679211

反应详情

EQUATION

反应方程式

HRID 1679211 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-(1-methanesulfonyloxyethylidene)acetate (1.12 g) in benzene (11 ml) is added morpholine (0.26 ml) under ice cooling, and the mixture is kept at 10° C overnight. The reaction mixture is washed with water, dried, and evaporated under reduced pressure. Purification of the obtained residue (1 g) by chromatograaphy over silica gel (10 g) using a mixture of benzene and ethyl acetate (1:2) gives p-nitrobenzyl α-[4-cyclopropylmethoxycarbonylthio-3-phenoxyacetamido-2-oxoazetidin-1-yl]-α-(1-morpholinoethylidene)acetate (602 mg). Foam. IR: νmaxCHCl3 3430, 1774, 1694br, 1604, 1105, cm-1. NMR: δCDCl3 0.22m5H, 2.27+2.24s3H, 3.43m4H, 3.77m4H, 4.02d(6.4Hz)2H, 4.57s2H, 5.05-5.27m3H, 5.89d(5.4Hz)1H, 4.12-7.65m7H, 8.23d(8.4Hz)2H.

WORKUP

后处理

  1. washThe reaction mixture is washed with water
  2. customdried
  3. customevaporated under reduced pressure
  4. customPurification of the obtained residue (1 g) by chromatograaphy over silica gel (10 g)
  5. additiona mixture of benzene and ethyl acetate (1:2)