HRID231575
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To approximately 2 ml of ethylene oxide cooled in an ice bath was added a suspension of 4-nitro-2H-1,2-benzisothiazol-3-one 1,1-dioxide (2.0 g, 8.76 mmol) in H2O (140 ml). After stirring in the ice bath for 1 hour, the mixture was allowed to stir at 20-25° for 18 hours. Water was removed under reduced pressure and the residue flash chromatographed over silica gel. Elution with 2% isopropanol-98% CH2Cl2 gave product which was recrystallized from EtOAc-hexane to give the 2-hydroxethyl derivative (0.39 g, 16%), m.p. 140-1°.
WORKUP
后处理
- additionwas added
- customWater was removed under reduced pressure
- customthe residue flash chromatographed over silica gel
- washElution with 2% isopropanol-98% CH2Cl2
- customgave product which
- customwas recrystallized from EtOAc-hexane
- customto give the 2-hydroxethyl derivative (0.39 g, 16%), m.p. 140-1°