HRID712417
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 suspension of 5-benzyltetrahydropyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione (3.88 g) in THF (80 mL) at −5° C. was added LiAlH4 (1.92 g) slowly. The reaction mixture was heated to reflux for 4 h, and then quenched with water, the mixture was extracted with EtOAc. The organic phase was dried over anhydrous Na2SO4 for 1 h and filtered. The filtrate was concentrated in vacuo and the residue was chromatographed with a silica gel column (eluting agent: 200:30:1 (v/v) DCM/MeOH/NH3H2O) to give the title compound as oil (2.07 g, 61.00%).
WORKUP
后处理
- temperatureThe reaction mixture was heated
- temperatureto reflux for 4 h
- customquenched with water
- extractionthe mixture was extracted with EtOAc
- dry with materialThe organic phase was dried over anhydrous Na2SO4 for 1 h
- filtrationfiltered
- concentrationThe filtrate was concentrated in vacuo
- customthe residue was chromatographed with a silica gel column (eluting agent: 200:30:1 (v/v) DCM/MeOH/NH3H2O)