HRID639104

反应详情

EQUATION

反应方程式

HRID 639104 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a solution of 1,1-dimethylethyl 3-cyano-4-oxo-1-pyrrolidinecarboxylate (3.9 g, 18.6 mmol) in acetone (185 mL) were added K2CO3 (3.07 g, 22.3 mmol) and MeI (1.39 mL, 22.3 mmol). After 12 h at reflux, the solution was cooled and the solid precipitate filtered. The filtrate was then concentrated and the residue purified by column chromatography (silica, 0.5% MeOH in DCM (1% NH4OH)) affording the title compound (2.3 g, 55%) as a yellow oil: LCMS (ES) m/e 225 (M+H)+.

WORKUP

后处理

  1. temperatureAfter 12 h at reflux
  2. temperaturethe solution was cooled
  3. filtrationthe solid precipitate filtered
  4. concentrationThe filtrate was then concentrated
  5. customthe residue purified by column chromatography (silica, 0.5% MeOH in DCM (1% NH4OH))