反应详情

温度

60 °C

A suspension of (S)-tert-butyl 2-(4-(diphenylmethyleneamino)phenyl)morpholine-4-carboxylate (54.1 g, 122 mmol), ammonium formate (116 g, 1.83 mol) and Pd/C 5% (6.5 g, 3.06 mmol) in methanol (930 ml) was stirred at 60° C. for 2 h. The reaction mixture was filtered and concentrated. The residue was dissolved in ethyl acetate and water. The organic phase was extracted twice with 0.5M HCl. The combined aqueous phases were basified with 2M-NaOH and extracted twice with DCM. The organic phases were dried over magnesium sulfate, filtered and dried in vacuo, to yield 31.95 g off-white solid. MS (ISP): 279.1 ([M+H]+).

1. filtrationThe reaction mixture was filtered
2. concentrationconcentrated
3. dissolutionThe residue was dissolved in ethyl acetate
4. extractionThe organic phase was extracted twice with 0.5M HCl
5. extractionextracted twice with DCM
6. dry with materialThe organic phases were dried over magnesium sulfate
7. filtrationfiltered
8. customdried in vacuo