HRID2238559

反应详情

EQUATION

反应方程式

HRID 2238559 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. washAmberlyst 15® (5.56 g, 26.1 mmol) was washed three times with methanol
  2. waitThe mixture was left
  3. customthe resin was removed by filtration (washing with methanol)
  4. concentrationThe combined methanol fractions were concentrated
  5. customto give a crude oil (1.62 g) which
  6. customwas purified by automated flash silica-gel column chromatography (Biotage SP4)
  7. washeluting with a 0-100% gradient of ethyl acetate in hexane