反应详情

Under ice cooling, sodium t-butoxide (1.96 g, 20.4 mmol) was added to a N,N-dimethylacetamide (30 mL) solution of 8-benzyloxy-1,3,3-trimethyl-1,5-dihydrobenzo[b][1,4]diazepine-2,4-dione (6.0 g, 18.5 mmol), and the mixture was stirred for 30 minutes. 1.63 mL (20.4 mmol) of ethyl iodide was added dropwise. The reaction solution was stirred at 10-20° C. for 4 hours. Water (42 mL) was added to the reaction solution, and the mixture was stirred at 10° C. or less for 30 minutes. Thereafter, precipitated crystals were collected by filtration, and the crystals were added to methanol (60 mL). The resultant was heated under reflux, and stirred at 10° C. or less for 30 minutes. Crystals were collected by filtration, then washed with methanol, and dried at 60° C., thereby obtaining 5.90 g of a white, powdery target compound (yield: 91%).

1. stirringThe reaction solution was stirred at 10-20° C. for 4 hours
2. stirringthe mixture was stirred at 10° C. or less for 30 minutes
3. customThereafter, precipitated crystals
4. filtrationwere collected by filtration
5. additionthe crystals were added to methanol (60 mL)
6. temperatureThe resultant was heated
7. temperatureunder reflux
8. stirringstirred at 10° C. or less for 30 minutes
9. filtrationCrystals were collected by filtration
10. washwashed with methanol
11. customdried at 60° C.