HRID744825

反应详情

EQUATION

反应方程式

HRID 744825 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

50 mg of tetrabutylammonium fluoride trihydrate are added to 115 mg of 5(S)-tert-butoxycarbonylamino-4(S)-tert-butyldimethylsilyloxy-7(S)-isopropyl-2(R)-methyl-8-[4-methoxy-3-(3-methoxy-propyloxy)-phenyl]-octanoic acid [N-(3-carbamoyl-propyl)]-amide in 4 ml of dimethylformamide at 0° C. The reaction mixture is stirred for a further 5 hours at room temperature and then concentrated by evaporation. 20 ml of saturated sodium hydrogen carbonate solution are added to the evaporation residue and the mixture is extracted repeatedly with ethyl acetate. The organic phases are washed with saturated sodium chloride solution and concentrated by evaporation. The residue is purified by means of FC (18 g of silica gel, dichloromethane/methanol=9:1). The title compound is obtained: Rf (dichloromethane/methanol=9:1): 0.24.

WORKUP

后处理

  1. concentrationconcentrated by evaporation
  2. addition20 ml of saturated sodium hydrogen carbonate solution are added to the evaporation residue
  3. extractionthe mixture is extracted repeatedly with ethyl acetate
  4. washThe organic phases are washed with saturated sodium chloride solution
  5. concentrationconcentrated by evaporation
  6. customThe residue is purified by means of FC (18 g of silica gel, dichloromethane/methanol=9:1)