HRID270118
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
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
- temperatureheated under nitrogen
- temperatureat reflux for 1 h
- concentrationThe mixture was concentrated to dryness
- custompurified by chromatography
- washeluting with a gradient from dichloromethane to 5% methanol in dichloromethane
- customby recrystallising twice from acetonitrile