反应详情

2-Chloro-9-cyclopentyl-7,7-difluoro-8,9-dihydro-5H-pyrimido[4,5-b][1,4]diazepin-6(7H)-one (100 g, 0.33 mol) was dissolved in DMA (700 mL) and cooled in ice bath under nitrogen. NaH (14.35 g, 60% in mineral oil, 0.363 mol) was added portionwise over a period of 20 min and the resulting mixture was continued to stir in ice bath for 10 min. Then iodomethane (21 mL, 0.363 mol) was added over a period of 10 min in ice bath and the mixture was stirred in ice bath for 10 min and then allowed to warm to room temperature and stirred for 1 h. The mixture was poured into ice water (2.5 L) and the resulting solid was filtered, washed with water, dried to give 98 g of 2-chloro-9-cyclopentyl-7,7-difluoro-5-methyl-8,9-dihydro-5H-pyrimido[4,5-b][1,4]diazepin-6(7H)-one.

1. temperaturecooled in ice bath under nitrogen
2. stirringthe mixture was stirred in ice bath for 10 min
3. stirringstirred for 1 h
4. filtrationthe resulting solid was filtered
5. washwashed with water
6. customdried