反应详情

A solution of 6.8 g (20 mmole) of 9-chloro-7-(2-chlorophenyl)-5H-pyrimido[5,4-d][2]benzazepine, 6 g (30 mmole) of 85% m-chloroperbenzoic acid in 200 ml of methylene chloride was stirred at room temperature for 4 hrs. The mixture was washed with an excess of ice cold dilute sodium hydroxide, dried over ahydrous sodium sulfate and filtered over hyflo. The filtrate was concentrated at reduced pressure to dryness. The residue was crystallized from a mixture of methylene chloride and ether to give a crude product, mp 228°-229° C. Recrystallization from a mixture of methylene chloride and ether gave the product, mp 216°-217° C.

1. washThe mixture was washed with an excess of ice cold dilute sodium hydroxide
2. dry with materialdried over ahydrous sodium sulfate
3. filtrationfiltered over hyflo
4. concentrationThe filtrate was concentrated at reduced pressure to dryness
5. customThe residue was crystallized from a mixture of methylene chloride and ether