反应详情

A mixture of 1.0 g (0.0028 mole) of 2-chloro-7,7-difluoro-5-methyl-9-(2-phenyl-cyclopropyl)-5,7,8,9-tetrahydro-pyrimido[4,5-b][1,4]diazepin-6-one (VII-287) and 0.55 g (0.0034 mole) of 4-amino-3-methoxy-benzoic acid in 6.4 mL of ethanol-water-hydrochloric acid (20:80:1) was refluxed for 18 hours, then cooled and partially concentrated under reduced pressure. The resulting solid was collected by filtration, washed with water and dried to give 0.97 g of 4-[7,7-difluoro-5-methyl-6-oxo-9-(trans-2-phenyl-cyclopropyl)-6,7,8,9-tetrahydro-5H-pyrimido[4,5-b][1,4]diazepin-2-ylamino]-3-methoxy-benzoic acid (I-287).

1. temperaturewas refluxed for 18 hours
2. temperaturecooled
3. concentrationpartially concentrated under reduced pressure
4. filtrationThe resulting solid was collected by filtration
5. washwashed with water
6. customdried