反应详情

There was dissolved 0.4 g of ethyl-α-(1-carboxyethyl)amino-γ-oxo-γ-phenylbutyrate prepared in Example 10 into 8.0 ml of 1.6% (v/v) H2SO4 -AcOH, to which 0.1 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, to which 2.5 ml of 1N NaOH solution was added and the resultant was concentrated under reduced pressure. After the residue was dissolved in water, the solution was adjusted to pH 3.0 and extracted with dichloromethane, the organic layer being washed with a saturated sodium chloride solution and concentrated under reduced pressure. The residue was crystallized from ethyl acetate to give 0.25 g of ethyl-α-(1-carboxyethyl)amino-γ-phenylbutyrate ((αS,1S)-form/(αR,1S)-form=99/1).

1. customthe hydrogenation reaction
2. customwas carried out at room temperature under atmospheric pressure
3. customAfter completion of the reaction
4. filtrationthe catalyst was filtered off with suction, to which 2.5 ml of 1N NaOH solution
5. additionwas added
6. concentrationthe resultant was concentrated under reduced pressure
7. dissolutionAfter the residue was dissolved in water
8. extractionextracted with dichloromethane
9. washthe organic layer being washed with a saturated sodium chloride solution
10. concentrationconcentrated under reduced pressure
11. customThe residue was crystallized from ethyl acetate