HRID651028

反应详情

EQUATION

反应方程式

HRID 651028 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

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

  1. concentrationthe mixture was concentrated to ca. 10 ml
  2. customThe organic layer was separated
  3. washwashed with water (100 ml)
  4. dry with materialdried (Na2SO4)
  5. customRemoval of the solvent
  6. customby evaporation
  7. customgave an crystalline residue, which
  8. customwas crystallized from ethanol/hexane