反应详情

To 5 ml of methylene chloride was added 462 mg (1.87 mmol) of (±)-3-(4-methoxybenzyl)-3,4-diazabicyclo[4.1.0]heptane-2,5-dione obtained in Reference Example 19. The mixture was cooled on a dry ice/ethanol bath, and 0.1 ml (1.1 mmol) of boron tribromide was added thereto dropwise. The temperature was elevated to room temperature, and the mixture was stirred for 2 hours. Water was added to the reaction mixture, and the mixture was extracted with ethyl acetate. The organic layer was dried over anhydrous sodium sulfate, the solvent was removed by distillation under reduced pressure, and the residue was recrystallized from ethanol/chloroform to obtain 120 mg (29.6%) of the titled compound.

1. customobtained in Reference Example 19
2. temperatureThe mixture was cooled on a dry ice/ethanol bath
3. customwas elevated to room temperature
4. extractionthe mixture was extracted with ethyl acetate
5. dry with materialThe organic layer was dried over anhydrous sodium sulfate
6. customthe solvent was removed by distillation under reduced pressure
7. customthe residue was recrystallized from ethanol/chloroform