HRID968472

反应详情

EQUATION

反应方程式

HRID 968472 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

2.57 ml of acetic acid, 5.32 ml of tributyltin hydride and 177 mg of bis(triphenyl phosphine) palladium(II) chloride were added to a solution of 9.58 g of ethyl 3-{[(allyloxy)-carbonyl]-amino}-3-{{3-{[(3-{[(propylamino)-carbonyl]-amino}-phenyl)-sulphonyl]-amino}-phenyl}}-propanoate from Example II.2.g in 245 ml of dichloromethane, and the resultant mixture was stirred at room temperature for 22 h. An aqueous solution of sodium bicarbonate was added, and the mixture was extracted with dichloromethane. After drying the organic phase over magnesium sulphate, the solvent was removed, and the crude product was purified by chromatography on silica gel (dichloromethane/methanol=10:1) to give 2.30 g of the desired compound.

WORKUP

后处理

  1. extractionthe mixture was extracted with dichloromethane
  2. dry with materialAfter drying the organic phase over magnesium sulphate
  3. customthe solvent was removed
  4. customthe crude product was purified by chromatography on silica gel (dichloromethane/methanol=10:1)