HRID2238559
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
Amberlyst 15® (5.56 g, 26.1 mmol) was washed three times with methanol and then a solution of 1-ethyl-3,3-dimethyl-5-{[(triphenylmethyl)oxy]methyl}-2-pyrrolidinone (1.08 g, 2.61 mmol) in methanol (50 ml) was added. The mixture was left to stand for 4 days at room temperature and then the resin was removed by filtration (washing with methanol). The combined methanol fractions were concentrated to give a crude oil (1.62 g) which was purified by automated flash silica-gel column chromatography (Biotage SP4), eluting with a 0-100% gradient of ethyl acetate in hexane, to give pure 1-ethyl-5-(hydroxymethyl)-3,3-dimethyl-2-pyrrolidinone (0.376 g) as an oil that solidified on standing.
WORKUP
后处理
- washAmberlyst 15® (5.56 g, 26.1 mmol) was washed three times with methanol
- waitThe mixture was left
- customthe resin was removed by filtration (washing with methanol)
- concentrationThe combined methanol fractions were concentrated
- customto give a crude oil (1.62 g) which
- customwas purified by automated flash silica-gel column chromatography (Biotage SP4)
- washeluting with a 0-100% gradient of ethyl acetate in hexane