反应详情

温度

80 °C

To a solution of [2-(4-nitro-phenyl)-ethyl]-carbamicacid tert-butyl ester (18.7 g, 70.30 mmol) in ethanol (200 ml) a slurry of 10% palladium on charcoal (2 g) in water (10 ml) was added. At 80° C. ammonium formate (44.3 g, 703 mmol) in water (90 ml) was added slowly. After complete addition the mixture was stirred at 80° C. for 1 h. The mixture was allowed to come to room temperature, filtered and concentrated in vacuo. The residue was diluted with water and extracted twice with dichloromethane. The combined organic layers were washed with water, dried over MgSO4, filtered and the solvent evaporated under reduced pressure to give the product as a yellow oil (13.5 g, 81%).

1. additionAfter complete addition the mixture
2. customto come to room temperature
3. filtrationfiltered
4. concentrationconcentrated in vacuo
5. additionThe residue was diluted with water
6. extractionextracted twice with dichloromethane
7. washThe combined organic layers were washed with water
8. dry with materialdried over MgSO4
9. filtrationfiltered
10. customthe solvent evaporated under reduced pressure