HRID49975
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
A solution of 5-benzyl-2-(3,5-dichlorophenyl)-tetrahydro-pyrrolo[3,4-c]pyrrole-1,3(2H,3aH)-dione (1.13 g, 3 mmol) in acetic acid (20 mL) was hydrogenated at atmospheric pressure over platinum oxide for 4 h. The catalyst was filtered off and the filtrate was poured into an ammonium hydroxide solution. The aqueous solution was extracted twice with methylene chloride. The organic layer was dried over sodium sulfate and concentrated in vacuo to give an oil (0.86 g) which was chromatographed over silica gel (CH2Cl2/MeOH/NH4OH: 90/9/1) to yield the above compound as a white solid (0.53 g). Mp=170° C. 1H NMR (DMSO-d6): 7.73 (1H, m), 7.47 (2H, m), 3.2-3.5 (4H, m), 2.8-2.9 (2H, m).
WORKUP
后处理
- filtrationThe catalyst was filtered off
- additionthe filtrate was poured into an ammonium hydroxide solution
- extractionThe aqueous solution was extracted twice with methylene chloride
- dry with materialThe organic layer was dried over sodium sulfate
- concentrationconcentrated in vacuo