反应详情

10% palladium carbon (1.66 g, water content: 54.8%) was added to an ethanol (150 mL) solution of 1-ethyl-7-benzyloxy-3,3,5-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (15.0 g, 42.6 mmol), and catalytic hydrogenation reaction was performed at 40-50° C., at 3 atm. The reaction solution was filtered to remove a catalyst, and ethanol was distilled off. Methanol (105 mL) and water (105 mL) were added to the resulting residue, and the mixture was heated while stirring. After the dissolution was confirmed, stirring under ice cooling was conducted for 1 hour, and precipitated crystals were collected by filtration. The resulting crystals were washed with 50% methanol (30 mL), and dried at 60° C., thereby obtaining 10.7 g of a white, powdery target compound (yield: 96%).

1. customwas performed at 40-50° C., at 3 atm
2. filtrationThe reaction solution was filtered
3. customto remove a catalyst, and ethanol
4. distillationwas distilled off
5. additionMethanol (105 mL) and water (105 mL) were added to the resulting residue
6. temperaturethe mixture was heated
7. dissolutionAfter the dissolution
8. stirringstirring under ice cooling
9. customprecipitated crystals
10. filtrationwere collected by filtration
11. washThe resulting crystals were washed with 50% methanol (30 mL)
12. customdried at 60° C.