反应详情

1-[1-(2-Toluoylmethyl)-2-oxo-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepin-3-yl]-3-(3-ethoxycarbonylphenyl)urea (500 mg) was suspended in 1,2-dichloroethane (10 ml), 2,2-dimethylbutyryl chloride (144 mg) and pyridine (86 μl ) were added, and the mixture was refluxed for one hour and 30 minutes. Water (100 ml) and ethyl acetate (100 ml) were added to the reaction mixture, separated, the organic layer was washed with 1N hydrochloric acid, and dried over anhydrous sodium sulfate. The solvent was evaporated under reduced pressure, the residue was purified by silica gel column chromatography(n-hexane:ethyl acetate=2:1), to thereby obtain 248 mg of the titled compound.

1. temperaturethe mixture was refluxed for one hour and 30 minutes
2. customseparated
3. washthe organic layer was washed with 1N hydrochloric acid
4. dry with materialdried over anhydrous sodium sulfate
5. customThe solvent was evaporated under reduced pressure
6. customthe residue was purified by silica gel column chromatography(n-hexane:ethyl acetate=2:1)