HRID2177792

反应详情

EQUATION

反应方程式

HRID 2177792 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

10% Palladium on carbon (0.05 g) was added to a solution of methyl 6-(benzenesulphonylmethyl)-2-(3-t-butyoxycarbonylamino-prop-1-yn-1-yl)-3-(furan-3-yl)benzoate (Intermediate 132, 0.22 g) in ethanol (10 ml) and THF (10 ml) and the mixture was stirred at room temperature in an atmosphere of hydrogen (balloon) for 60 hours. The mixture was filtered through Celite and the filtrate was evaporated to dryness. The residue was purified by chromatography on silica eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 25-60% to give methyl 6-(benzenesulphonylmethyl)-2-(3-t-butoxycarbonylaminopropyl)-3-(furan-3-yl)benzoate (0.115 g) as a colourless gum.

WORKUP

后处理

  1. filtrationThe mixture was filtered through Celite
  2. customthe filtrate was evaporated to dryness
  3. customThe residue was purified by chromatography on silica eluting with a mixture of ethyl acetate and cyclohexane with a gradient of 25-60%