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 50° 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 50°
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