反应详情

4M HCl/dioxane (5.49 mL, 22.0 mmol) was added to a solution of (S)-3-(tert-butoxycarbonylamino)-2-(4-chlorophenyl)propanoic acid (0.329 g, 1.10 mmol) in 2:1 dioxane:DCM (10 mL). The reaction mixture was stirred at room temperature overnight (16 hours), after which it was concentrated to 1/3 volume. The resulting cloudy mixture was diluted with ether, and the mixture was concentrated again to 1/3 volume. The mixture was diluted again with ether (20 mL), and the solids were isolated by filtration through a medium frit funnel with nitrogen pressure. The solids were rinsed with ether (5×10 mL), dried under nitrogen pressure, and dried in vacuo to give (S)-3-amino-2-(4-chlorophenyl)propanoic acid hydrochloride (0.199 g, 76.8% yield) as a white powder. HPLC>99 area % pure. LC/MS (APCI+) m/z 200.

1. concentrationafter which it was concentrated to 1/3 volume
2. additionThe resulting cloudy mixture was diluted with ether
3. concentrationthe mixture was concentrated again to 1/3 volume
4. additionThe mixture was diluted again with ether (20 mL)
5. customthe solids were isolated by filtration through a medium frit funnel with nitrogen pressure
6. washThe solids were rinsed with ether (5×10 mL)
7. customdried under nitrogen pressure
8. customdried in vacuo