HRID651028
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 the ethyl 3-[bis(methylsulfonyl)amino]-6-chloro-2-(3-chlorobenzoyl)-1H-indole-1-carboxylate (step 1, 532 mg, 0.998 mmol) in ethanol (15 ml) was added a solution of potassium hydroxide (395 mg, 5.99 mmol) in water (8 ml) at room temperature. After stirring for 1 h at ambient temperature, the mixture was concentrated to ca. 10 ml, and partioned between with ethyl acetate (150 ml) and water (100 ml). The organic layer was separated and washed with water (100 ml), and dried (Na2SO4). Removal of the solvent by evaporation gave an crystalline residue, which was crystallized from ethanol/hexane to afford 182 mg (48%) of the title compound.
WORKUP
后处理
- concentrationthe mixture was concentrated to ca. 10 ml
- customThe organic layer was separated
- washwashed with water (100 ml)
- dry with materialdried (Na2SO4)
- customRemoval of the solvent
- customby evaporation
- customgave an crystalline residue, which
- customwas crystallized from ethanol/hexane