反应详情

In a saturated aqueous solution of sodium hydrogencarbonate was dissolved (S)-3-(3-t-butoxycarbonylaminopropyl)-2-oxopiperazine-1-acetic acid t-butyl ester oxalate (1.6 g, 3.47 mmol). The solution was subjected to extraction with ethyl acetate, and the extract solution was concentrated under reduced pressure. The concentrate and N-Z-Gly-OH (0.87 g, 4.16 mmol) were dissolved in 16.0 cc of acetone. To the solution was added, at 15° C. under stirring, 1-ethyl-3-(3-dimethylaminopropyl)carbodiimide hydrochloride (0.87 g, 4.51 mmol). The mixture was stirred for one hour at room temperature, and the reaction mixture was concentrated under reduced pressure. The concentrate was washed with a 5% aqueous solution of potassium hydrogensulfate and a saturated aqueous solution of sodium hydrogencarbonate. The organic layer was concentrated under reduced pressure, and the concentrate was purified by means of a silica gel column chromatography (ethyl acetate) to afford 1.95 g (100%) of the titled compound as a colorless amorphous powdery product.

1. extractionThe solution was subjected to extraction with ethyl acetate
2. concentrationthe extract solution was concentrated under reduced pressure
3. concentrationThe concentrate
4. additionTo the solution was added, at 15° C.
5. stirringThe mixture was stirred for one hour at room temperature
6. concentrationthe reaction mixture was concentrated under reduced pressure
7. washThe concentrate was washed with a 5% aqueous solution of potassium hydrogensulfate
8. concentrationThe organic layer was concentrated under reduced pressure
9. customthe concentrate was purified by means of a silica gel column chromatography (ethyl acetate)