反应详情

温度

60 °C

A round bottom flask was charged with sodium hydride (0.295 g, 7.46 mmol) in 9.0 mL of DMF and treated with 5,7-dihydro-6H-dibenz[b,d]azepin-6-one (1.3 g, 6.22 mmol) (CAS #20011-90-9, prepared as described in Brown, et. al., Tetrahedron Letters, No. 8, 667-670, (1971) and references cited therein, which are incorporated herein by reference). After stirring at 60° C. for 1 hour, the solution was treated with methyl iodide (1.16 mL, 18.6 mmol) and stirring continued for 17 hours with the exclusion of light. After cooling, the reaction was diluted with CH2Cl2/H2O, washed with NaHSO4 solution, H2O, and dried over Na2SO4. Evaporation and flash chromatography (SiO2, CHCl3) gave 0.885 g (63%) of the title compound as a colorless solid.

1. customprepared
2. stirringstirring
3. waitcontinued for 17 hours with the exclusion of light
4. temperatureAfter cooling
5. washwashed with NaHSO4 solution, H2O
6. dry with materialdried over Na2SO4
7. customEvaporation and flash chromatography (SiO2, CHCl3)