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 (400 mg) obtained from Step 1 of Example 93 was suspended in 1,2-dichloroethane (10 ml), isovaleryl chloride (104 μl) and pyridine (70 μl) were added, and the mixture was refluxed for 1 hour and 30 minutes. Water and methylene chloride were added to the reaction mixture, separated, and the organic layer was successively washed with 1N hydrochloric acid and saturated aqueous sodium bicarbonate, 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 296 mg of the titled compound.

1. temperaturethe mixture was refluxed for 1 hour and 30 minutes
2. customseparated
3. washthe organic layer was successively washed with 1N hydrochloric acid and saturated aqueous sodium bicarbonate
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)