反应详情

1,1′-Carbonyldiimidazole (244 mg) was added to a solution of 1-(2-toluoylmethyl)-2-oxo-3-amino-5-pivaloyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (393 mg) in anhydrous tetrahydrofuran (5 ml), stirred for 30 minutes at room temperature,N,N-dimethyl-m-phenylenediamine dihydrochloride (335 mg) and triethylamine (0.67 ml) was added, and the mixture was refluxed overnight. The reaction mixture was concentrated under reduced pressure, appeared insoluble material was removed and purified by silica gel column chromatography (n-hexane:ethyl acetate=1:1). Etanol was added to the residue for crystallization and filtrated, to thereby obtain 224 mg of the title compound (Yield: 40.3%) as white solid.

1. additionwas added
2. temperaturethe mixture was refluxed overnight
3. concentrationThe reaction mixture was concentrated under reduced pressure
4. customwas removed
5. custompurified by silica gel column chromatography (n-hexane:ethyl acetate=1:1)
6. additionEtanol was added to the residue for crystallization
7. filtrationfiltrated