HRID639105
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 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
- concentrationthe solution was concentrated
- customthe residue partitioned between H2O-DCM
- washThe aqueous phase was washed several times with DCM
- dry with materialthe combined organic fractions were dried (Na2SO4)
- concentrationconcentrated
- custompurified by column chromatography (silica, 1% MeOH in DCM (1% NH4OH))