反应详情

(2S)-2-[(tert-butoxycarbonyl)amino]-3-(3,5-difluorophenyl)propanoic acid methyl ester (II, EXAMPLE 1, 0.60 g (0.002 moles, 1 equivalent), methanol (20 mL) and hydrochloric acid (3N, 20 mL) are mixed. The mixture is then heated to 500 and stirred until complete as measured by HPLC. When the reaction is complete, the contents are cooled to 20-25° and the pH of the mixture is adjusted to 8 with saturated sodium bicarbonate and then concentrated under reduced pressure. This mixture is extracted with ethyl acetate (2×20 mL) and the combined organic phases are dried over sodium sulfate, filtered and concentrated, HPLC (Retention time=2.89 min; Zorbax RX-C8 acetonitrile/0.05M potassium dihydrogen phosphate, 60/40; 1.0 mL/min, λ=210 nm.

1. temperatureThe mixture is then heated to 500
2. temperaturethe contents are cooled to 20-25°
3. concentrationconcentrated under reduced pressure
4. extractionThis mixture is extracted with ethyl acetate (2×20 mL)
5. dry with materialthe combined organic phases are dried over sodium sulfate
6. filtrationfiltered
7. concentrationconcentrated