HRID530431

反应详情

EQUATION

反应方程式

HRID 530431 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To the solution of 2-(3-aminophenyl)-1H-indole-1-carboxamide (50.2 mg, 0.2 mmol, 1 eq) in anhydrous THF (2 mL) was added 3-ethylphenyl isocyanate (29 μL, 1 eq) and the reaction solution was stirred at room temperature for one hour. It was then diluted with ethyl acetate, washed with aqueous ammonium chloride, saturated aqueous sodium bicarbonate, brine, and lastly dried with anhydrous sodium sulfate. The upper solution was decanted, concentrated and the oily residue was subject to a gradient column chromatography (from EtOAc-Hex 1:2 to MeOH-EtOAc 1:10). The product fractions were collected, concentrated, and the solid residue was triturated with EtOAc-Hex (1:1) to give 2-[3-({[(3-ethylphenyl)amino]carbonyl}amino)phenyl]-1H-indole-1-carboxamide as white solid upon filtration in amount of 32 mg.

WORKUP

后处理

  1. washwashed with aqueous ammonium chloride, saturated aqueous sodium bicarbonate, brine
  2. dry with materiallastly dried with anhydrous sodium sulfate
  3. customThe upper solution was decanted
  4. concentrationconcentrated
  5. customThe product fractions were collected
  6. concentrationconcentrated
  7. customthe solid residue was triturated with EtOAc-Hex (1:1)