HRID651008
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 stirred solution of ethyl 2-benzoyl-6-chloro-3-[(methoxycarbonyl)amino]-1H-indole-1-caboxylate (step 3, 680 mg, 1.7 mmol) in ethanol (20 ml) was added 2N aqueous KOH (10 ml) at room temperature. After stirring for 2 h, the mixture was concentrated and extracted with dichloromethane (50 ml×2). The combined organic layers were dried (MgSO4) and concentrated to give an crystalline residue. Recrystallization from ethyl acetate/hexane afforded 320 mg (57%/o) of the title compound as yellow solids.
WORKUP
后处理
- concentrationthe mixture was concentrated
- extractionextracted with dichloromethane (50 ml×2)
- dry with materialThe combined organic layers were dried (MgSO4)
- concentrationconcentrated
- customto give an crystalline residue
- customRecrystallization from ethyl acetate/hexane