HRID749258

反应详情

EQUATION

反应方程式

HRID 749258 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

PROCEDURE

实验过程

A solution of 3-(3-{[7-(benzyl{(2R)-2-[8-(benzyloxy)-2-oxo-1,2-dihydroquinolin-5-yl]-2-hydroxyethyl}amino)heptyl]oxy}propyl)benzenesulfonamide (36 mg) in ethanol (10 ml) with ethyl acetate (2 ml) and glacial acetic acid (1 ml) was hydrogenated using 10% palladium on carbon (50% water by weight, 10 mg) and 20% palladium hydroxide on carbon (10 mg) for 19 h. The catalyst was removed by filtration and the filtrate was evaporated in vacuo. The residue was purified on an aminopropyl SPE cartridge (2 g), eluting with methanol-dichloromethane mixtures. Evaporation of the appropriate fractions with glacial acetic acid gave the title compound (15 mg). LCMS RT=2.26 min ES+ve m/z 532 (MH)+

WORKUP

后处理

  1. customfor 19 h
  2. customThe catalyst was removed by filtration
  3. customthe filtrate was evaporated in vacuo
  4. customThe residue was purified on an aminopropyl SPE cartridge (2 g)
  5. washeluting with methanol-dichloromethane mixtures
  6. customEvaporation of the appropriate fractions with glacial acetic acid