HRID2231604

反应详情

EQUATION

反应方程式

HRID 2231604 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
60 °C

PROCEDURE

实验过程

To a mixture of 8 ml of acetic acid and 2 ml of water is added 1.0 g of 2,2-dimethyl-7-azido-1-aza-3-oxa-bicyclo[4,2,0]octane-8-one (1:4 cis-trans mixture) and the mixture is stirred at 60° C. for 4 hours and concentrated to dryness. Tetrahydrofuran (15 ml) is added and the insoluble matter is filtered off. The filtrate is concentrated to dryness and the residue is dissolved in a small amount of chloroform and subjected to column chromatography using silica gel (20 g), elution being carried out with chloroform-ethyl acetate (1:1) and ethyl acetate in that order to give 179 mg of 3-azido-4-hydroxyethyl-2-azetidinone as a colorless oil.

WORKUP

后处理

  1. concentrationconcentrated to dryness
  2. additionTetrahydrofuran (15 ml) is added
  3. filtrationthe insoluble matter is filtered off
  4. concentrationThe filtrate is concentrated to dryness
  5. dissolutionthe residue is dissolved in a small amount of chloroform
  6. washsilica gel (20 g), elution