HRID1241524

反应详情

EQUATION

反应方程式

HRID 1241524 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

4-Nitrobenzyl (5R,6S)-6-[(1R)-1-hydroxyethyl]-3-{4-[(methylamino)carbonyl]phenyl}-7-oxo-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylate (60 mg) obained in the above Step b) was dissolved in THF (6 ml) and ion-exchange water (4.7 ml), and thereto was added 0.1 N aqueous sodium hydrogen carbonate solution (1.3 ml). To the mixture was added 10% palladium on carbon (120 mg), and the mixture was subjected to hydrogenolysis for 30 minutes under atmospheric pressure at room temperature. The catalyst was removed by filtration, and washed with water, and chloroform was added to the filtrate, and extracted and separated (three times). The organic solvent in the aqueous layer was removed under reduced pressure, and the resultant was purified by polymer chromatography (CHP-20P). The fractions eluted with 0–2% aqueous THF solution were combined and lyophilized to give (5R,6S)-6-[(1R)-1-hydroxyethyl]-3-{4-[(methylamino)carbonyl]-phenyl}-7-oxo-1-azabicyclo[3.2.0]hept-2-ene-2-carboxylic acid sodium salt (18 mg).

WORKUP

后处理

  1. customThe catalyst was removed by filtration
  2. washwashed with water, and chloroform
  3. additionwas added to the filtrate
  4. extractionextracted
  5. customseparated (three times)
  6. customThe organic solvent in the aqueous layer was removed under reduced pressure
  7. customthe resultant was purified by polymer chromatography (CHP-20P)
  8. washThe fractions eluted with 0–2% aqueous THF solution