反应详情

温度

50 °C

Methyl N-{[(3R)-4-(phenylmethyl)-3-morpholinyl]carbonyl}-D-serinate (D48, 3.72 g, 11.55 mmol) was dissolved in EtOH (50 mL), treated with 10% Pd on C (450 mg) then placed under an atmosphere of hydrogen over the weekend. Left stirring for further 6 hours. Added 10% Pd on C (200 mg) and left under an atmosphere of hydrogen overnight. Catalyst removed by filtration through kieselguhr washed with acid, washing well with EtOH. Solvent removed under reduced pressure to afford a colourless oil. Oil dissolved in dry MeOH (15 mL) and heated at 50° C. overnight. Left heating for a further 3 hours before cooling to R.T. Solvent removed under reduced pressure. Residue triturated with DCM to afford the title compound as an off white solid in 35% yield over the 2 steps.

1. waitLeft
2. waitleft under an atmosphere of hydrogen overnight
3. customCatalyst removed by filtration through kieselguhr
4. washwashed with acid
5. washwashing well with EtOH
6. customSolvent removed under reduced pressure
7. customto afford a colourless oil
8. waitLeft
9. temperatureheating for a further 3 hours
10. temperaturebefore cooling to R.T
11. customSolvent removed under reduced pressure
12. customResidue triturated with DCM