HRID1099323

反应详情

EQUATION

反应方程式

HRID 1099323 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Carbonic acid (2S,4S)-2-tert-butylcarbonylamino-4-[4-methoxy-3-(3-methoxy-propoxy)-benzoyl]-5-methyl-hexylester tert-butyl ester (2.67 g) is dissolved in 25 mL of a mixture of ethanol/acetic acid, 2/1 at room temperature. Palladium metal, 10% on charcoal (0.3 g) is added and the suspension placed under an atmosphere of hydrogen at a pressure of 5 bar. Hydrogenation is continued for 3 days at 50° C. with periodic addition of more catalyst. The reaction mixture is filtered and the solvent removed to give an oil. The oil is purified by chromatography on silica-gel eluting with hexane/ethyl acetate mixtures. The product fractions are combined and the solvent is removed to give the title compound as an oil.

WORKUP

后处理

  1. additionHydrogenation is continued for 3 days at 50° C. with periodic addition of more catalyst
  2. filtrationThe reaction mixture is filtered
  3. customthe solvent removed
  4. customto give an oil
  5. customThe oil is purified by chromatography on silica-gel
  6. washeluting with hexane/ethyl acetate mixtures
  7. customthe solvent is removed