反应详情

[1,1′-Biphenyl]-4-yl-(5,11-dihydro-10H-dibenzo[b,e][1,4]diazepin-10-yl)methanone of Example 6 (0.97 g) was added to sodium hydride (2 equivalents, 60% in oil, washed with hexane) and N,N-dimethylformamide (25 mL). Iodomethane (0.45 g) was added and after overnight stirring, the mixture was poured into brine. The precipitate was collected, redissolved in dichloromethane and the solution filtered through a short column of Magnesol®. The column was rinsed with several volumes of dichloromethane, and the combined eluate refluxed with the gradual addition of hexane until incipient crystallization. Cooling and filtration provided the title compound (0.89 g), m.p. 198-201° C.

1. customThe precipitate was collected
2. dissolutionredissolved in dichloromethane
3. filtrationthe solution filtered through a short column of Magnesol®
4. washThe column was rinsed with several volumes of dichloromethane
5. temperaturethe combined eluate refluxed with the gradual addition of hexane until incipient crystallization
6. temperatureCooling
7. filtrationfiltration