反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
To a stirred solution of 4.2 g of (3R)-3-{[4-{(5R)-5-azidomethyl-2-oxo-oxazolidin-3-yl}-2-fluoro-phenyl]-benzyl-oxycarbonyl-amino}-pyrrolidine-1-carboxylic acid tert-butyl ester (7.3 mmol) in 50 ml ethyl acetate were added 400 mg of Pd/C 10% and the mixture was stirred under hydrogen over night. The reaction was controlled by TLC. The Pd/C was filtered, the filtrate evaporated to dryness. The residue was dissolved in 5 ml acetic acid and 2 ml acetic anhydride was added. The reaction was stirred at rt for 2 hrs and monitored by TLC. The solvents were evaporated, the residue dissolved in ethyl acetate, washed with water and brine, dried over Mg sulfate, filtered and the filtrate evaporated to dryness.
WORKUP
后处理
- filtrationThe Pd/C was filtered
- customthe filtrate evaporated to dryness
- dissolutionThe residue was dissolved in 5 ml acetic acid
- addition2 ml acetic anhydride was added
- stirringThe reaction was stirred at rt for 2 hrs
- customThe solvents were evaporated
- dissolutionthe residue dissolved in ethyl acetate
- washwashed with water and brine
- dry with materialdried over Mg sulfate
- filtrationfiltered
- customthe filtrate evaporated to dryness