HRID491785

反应详情

EQUATION

反应方程式

HRID 491785 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

Trans-5-methoxycarbonyl-3-[4-(methylamino)cyclohexylcarbonylamino]-N-(5-chloropyridin-2-yl)benzofuran-2-carboxamide hydrochloride (1.50 g) obtained in Example 218 is suspended in dichloromethane (80 ml), and thereto are added acetyl chloride (307 μl) and triethylamine (1.60 ml) under ice-cooling. The mixture is warmed to room temperature, and stirred for 2 hours. To the reaction solution is poured a saturated aqueous sodium hydrogen carbonate solution, and the mixture is extracted with chloroform, washed with water and a saturated brine, and dried over sodium sulfate. The solvent is evaporated under reduced pressure, and the resulting residue is purified by NH-silica gel column chromatography (eluent: chloroform) to give the title compound (1.51 g).

WORKUP

后处理

  1. temperaturecooling
  2. extractionthe mixture is extracted with chloroform
  3. washwashed with water
  4. dry with materiala saturated brine, and dried over sodium sulfate
  5. customThe solvent is evaporated under reduced pressure
  6. customthe resulting residue is purified by NH-silica gel column chromatography (eluent: chloroform)