反应详情

Ethyl 3-aminobenzoate (373 mg) was dissolved in tetrahydrofuran (60 ml), under ice-cooling triphosgene (225 mg) was added, triethylamine (194 μl) was added thereto five times every 3 minutes, a solution of 1-(2-toluoylmethyl)-2-oxo-3-amino-5-(furan-2-ylcarbonyl)-8-methyl-1,3,4,5-tetrahydro-2H-1,5-benzodiazepine (856 mg) in tetrahydrofuran (15 ml) was added thereto, the mixture was allowed to come to room temperature and stirred overnight. The reaction mixture was concentrated under reduced pressure, water (50 ml) was added to the residue, extracted with methylene chloride. The organic layer was dried over anhydrous sodium sulfate, the solvent was evaporated under reduced pressure, and the residue was purified by silica gel column chromatography(chloroform:ethyl acetate=10:1), to thereby obtain 447 mg of the titled compound.

1. additionwas added
2. customto come to room temperature
3. concentrationThe reaction mixture was concentrated under reduced pressure, water (50 ml)
4. additionwas added to the residue
5. extractionextracted with methylene chloride
6. dry with materialThe organic layer was dried over anhydrous sodium sulfate
7. customthe solvent was evaporated under reduced pressure
8. customthe residue was purified by silica gel column chromatography(chloroform:ethyl acetate=10:1)