反应详情

温度

60 °C

A suspension of (S)-tert-Butyl 2-(4-(diphenylmethyleneamino)phenyl)morpholine-4-carboxylate (54.1 g), ammonium formate (116 g) and 5% palladium on charcoal (6.5 g) in methanol (930 ml) was stirred at 60° C. for 2 h. The reaction mixture was filtered and concentrated in vacuo. The residue was dissolved in ethyl acetate and water. The organic phase was extracted twice with 0.5 M aq. HCl. The combined aqueous phases were basified with 2 M aq. NaOH and extracted twice with dichloromethane. The organic phases were dried over magnesium sulfate, filtered and dried in vacuo to yield (S)-tert-butyl 2-(4-aminophenyl)morpholine-4-carboxylate (31.95 g, 94%) as an off-white solid. MS (ISP): 279.1 ([M+H]+).

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