HRID235754

反应详情

EQUATION

反应方程式

HRID 235754 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

CONDITIONS

反应条件

温度
65 °C

PROCEDURE

实验过程

A solution of (6R, 7S)-2,2-dimethyl-7-(1-methoxy-1-methylethyl)-1-aza-3-oxabicyclo[4.2.0]octan-8-one (142.3 mg) in a mixture of acetic acid (2.28 ml) and water (0.57 ml) was heated at 65° C. for 1.5 hours. The mixture was cooled to ambient temperature and then evaporated in vacuo. Xylene was added to the residue and the resultant suspension was evaporated in vacuo. The residue was dissolved in a mixture of methanol and xylene, and the resultant solution was evaporated in vacuo. This operation was repeated once and the residue was chromatographed on silica gel (1.5 g) eluting with a mixture of methylene chloride and acetone (10:1 to 1:1) to give (3S, 4R)-4-(2-hydroxyethyl)-3-(1-methoxy-1-methylethyl)azetidin-2-one (111.3 mg).

WORKUP

后处理

  1. temperatureThe mixture was cooled to ambient temperature
  2. customevaporated in vacuo
  3. additionXylene was added to the residue
  4. customthe resultant suspension was evaporated in vacuo
  5. dissolutionThe residue was dissolved in a mixture of methanol and xylene
  6. customthe resultant solution was evaporated in vacuo
  7. customthe residue was chromatographed on silica gel (1.5 g)
  8. washeluting with a mixture of methylene chloride and acetone (10:1 to 1:1)