反应详情

温度

46 °C

(S)-tert-Butyl 3-(3-cyanophenyl)-1-((4-methoxyphenyl)(methyl)amino)-1-oxopropan-2-ylcarbamate (2.7 g, 6.60 mmole) was dissolved in pyridine (18.6 ml) and acetic acid (9.3 ml). Raney Nickel (2.7 g of a slurry in H2O) was added and the resulting suspension was stirred at 46° C. overnight. The reaction was confirmed complete by reverse phase HPLC/MS. The reaction was cooled to room temperature and then filtered through celite. The filtrate was concentrated under reduced pressure and then partitioned between EtOAc and H2O. The aqueous layer was extracted with EtOAc (3×). The combined organics were washed with H2O (2×) and brine (2×). The organic layer was dried over MgSO4, filtered and concentrated. The crude produce was dried under high vacuum overnight and used without further purification. Yield was 2.70 g. MS (m/z) 413 [M+H]+.

1. temperatureThe reaction was cooled to room temperature
2. filtrationfiltered through celite
3. concentrationThe filtrate was concentrated under reduced pressure
4. custompartitioned between EtOAc and H2O
5. extractionThe aqueous layer was extracted with EtOAc (3×)
6. washThe combined organics were washed with H2O (2×) and brine (2×)
7. dry with materialThe organic layer was dried over MgSO4
8. filtrationfiltered
9. concentrationconcentrated
10. customThe crude produce
11. customwas dried under high vacuum overnight
12. customused without further purification