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
There was dissolved 0.20 g of ethyl-α-(1-carboxyethyl)amino-γ-oxo-γ-phenylbutyrate prepared in Example 10 into 11.0 ml of 1% (v/v) H2SO4 -EtOH, to which 0.05 g of 10% Pd/C was added and the hydrogenation reaction was carried out at room temperature under atmospheric pressure. After completion of the reaction, the catalyst was filtered off with suction and the ethanol solution was neutralized with sodium hydroxide, followed by distillation of the solvent under reduced pressure. The residue was dissolved in water and extracted with dichloromethane, the organic layer being concentrated under reduced pressure. The residue was crystallized from ethyl acetate to give 0.152 g of ethyl-α-(1-carboxyethyl)amino-γ-phenylbutyrate ((αS,1S)-form/(αR,1S)-form=99/1).
WORKUP
后处理
- customthe hydrogenation reaction
- customwas carried out at room temperature under atmospheric pressure
- customAfter completion of the reaction
- filtrationthe catalyst was filtered off with suction
- distillationfollowed by distillation of the solvent under reduced pressure
- dissolutionThe residue was dissolved in water
- extractionextracted with dichloromethane
- concentrationthe organic layer being concentrated under reduced pressure
- customThe residue was crystallized from ethyl acetate