反应详情

A mixture of 3.0 g of 8-chloro-5-(4-chlorophenyl)-5H-indeno[1,2-d]pyrimidin-5-ol in 15 ml of acetonitrile and 50 ml of methanesulfonic acid were stirred for approximately 18 hours. The reaction mixture was added to a large excess of a potassium bicarbonate solution and the resulting mixture was extracted with ethyl acetate. The organic layer was washed with a saturated sodium chloride solution, dried over magnesium sulfate, and concentrated in vacuo. Crystallization from acetonitrile/water provided 2.53 g of the desired title product, m.p. 238°-241° C. Two further recrystallizations provided material with a melting point of 245°-248° C.

1. extractionthe resulting mixture was extracted with ethyl acetate
2. washThe organic layer was washed with a saturated sodium chloride solution
3. dry with materialdried over magnesium sulfate
4. concentrationconcentrated in vacuo
5. customCrystallization from acetonitrile/water