HRID639105

反应详情

EQUATION

反应方程式

HRID 639105 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-3-methyl-4-oxo-1-pyrrolidinecarboxylate (2.3 g, 10.2 mmol) in EtOH (100 mL) at 0° C. was added NaBH4 (775 mg, 20.5 mmol) portion-wise. After 30 min., the solution was concentrated and the residue partitioned between H2O-DCM. The aqueous phase was washed several times with DCM and the combined organic fractions were dried (Na2SO4), concentrated and purified by column chromatography (silica, 1% MeOH in DCM (1% NH4OH)) affording the title compound as a yellow oil: LCMS (ES) m/e 227 (M+H)+.

WORKUP

后处理

  1. concentrationthe solution was concentrated
  2. customthe residue partitioned between H2O-DCM
  3. washThe aqueous phase was washed several times with DCM
  4. dry with materialthe combined organic fractions were dried (Na2SO4)
  5. concentrationconcentrated
  6. custompurified by column chromatography (silica, 1% MeOH in DCM (1% NH4OH))