HRID270118

反应详情

EQUATION

反应方程式

HRID 270118 的结构方程式

PROCEDURE

实验过程

A solution of 2-[[(2R)-3-Chloro-2-hydroxy-2-methylpropyl]oxy]-1H-isoindole-1,3 (2H)-dione (3.3 g, 12.2 mmol) in methanol (25 ml) was treated with triethylamine (3.4 ml) and heated under nitrogen at reflux for 1 h. The mixture was concentrated to dryness and purified by chromatography eluting with a gradient from dichloromethane to 5% methanol in dichloromethane. The chiral purity of the product was enhanced by recrystallising twice from acetonitrile to give the sub-title compound as a colourless solid (1.92 g).

WORKUP

后处理

  1. temperatureheated under nitrogen
  2. temperatureat reflux for 1 h
  3. concentrationThe mixture was concentrated to dryness
  4. custompurified by chromatography
  5. washeluting with a gradient from dichloromethane to 5% methanol in dichloromethane
  6. customby recrystallising twice from acetonitrile