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 5% Pd/C (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 0.5 M HCl. The combined aqueous phases were basified with 2 M 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 0.5 M HCl
5. extractionextracted twice with DCM
6. dry with materialThe organic phases were dried over magnesium sulfate
7. filtrationfiltered
8. customdried in vacuo