反应详情

A suspension of 4-(3,5-dichloro-pyridin-4-ylmethyl)-7-difluoromethoxy-2H-phthalazin-1-one (6.64 g, 17.8 mmoles), prepared as described in example 98, in acetonitrile (70 ml), under N2, was added with POCl3 (8.3 ml, 89 mmoles). After 4.5 hours under reflux and 1 night to stand, the mixture was dried under vacuum, taken up in CH2Cl2 and washed with an aqueous Na2CO3 solution, then discoloured with charcoal, filtered over celite and dried again to give 6.8 g of the title compound (yield: 97%).

1. customprepared
2. temperatureAfter 4.5 hours under reflux and 1 night
3. customthe mixture was dried under vacuum
4. washwashed with an aqueous Na2CO3 solution
5. filtrationfiltered over celite
6. customdried again