反应详情

To a suspension of 50% sodium hydride (48 mg; 1 mmole) in dimethylformamide (5 ml) cooled at 0°-5° C. was added dropwise a solution of 7-chloro-1,3,4,5-tetrahydro-3-(methoxycarbonyl)-1-(methoxymethyl)-4-(4-methoxyphenyl)-2H-1-benzazepin-2-one (102 mg; 0.25 mmole) in dimethylformamide (1 ml). After stirring at 0°-5° C. for 20 minutes, allyl bromide (360 μl ; 4 mmole) was added dropwise, and the reaction mixture was allowed to stir at 0° C. to room temperature for two hours. Excess sodium hydride was destroyed with water, and the mixture was extracted with ether. The aqueous layer was extracted with ether (two times), and the combined organic layers were dried (magnesium sulfate) and concentrated. The crude residue was triturated with hexane (20 ml) to obtain 93 mg of white, crystalline title compound. [The mother liquor contained additional product].

1. temperaturecooled at 0°-5° C.
2. stirringto stir at 0° C. to room temperature for two hours
3. customExcess sodium hydride was destroyed with water
4. extractionthe mixture was extracted with ether
5. extractionThe aqueous layer was extracted with ether (two times)
6. dry with materialthe combined organic layers were dried (magnesium sulfate)
7. concentrationconcentrated
8. customThe crude residue was triturated with hexane (20 ml)