反应详情

To 4-(2,3-diaminobenzoyl)amino-3-methoxy-N-methyl-N-[4-methyl-2-[5-(4-methylpiperazin-1-yl)carbonylpent-1-yloxy]phenyl]benzamide (120 mg) were added acetic acid (47 mg) and water (0.5 ml) and the suspension was stirred at ambient temperature until a clear solution was obtained. After being cooled to 5° C. a cold solution of sodium nitrite (15 mg) in water (0.3 ml) was added all at once to the solution. The reaction mixture as stirred at 5° C. for 5 minutes and then the temperature was raised to 75° C. and stirred for 10 minutes. The reaction mixture was cooled to 20° C. and the solution was stirred in an ice water bath for 1 hour. To the reaction mixture were added saturated aqueous sodium bicarbonate solution and chloroform and the organic layer was separated. The organic layer was washed with saturated aqueous sodium bicarbonate solution and brine and dried over magnesium sulfate. The solvent was evaporated and the residue was purified by preparative thin-layer chromatography (chloroform-methanol=10:1) to give 4-(1H-benzotriazol-4-yl)carbonylamino-3-methoxy-N-methyl-N-[4-methyl-2-[5-(4-methylpiperazin-1-yl)carbonylpent-1-yloxy]phenyl]benzamide (81 mg) to give a powder.

1. customwas obtained
2. additionwas added all at once to the solution
3. stirringThe reaction mixture as stirred at 5° C. for 5 minutes
4. temperaturethe temperature was raised to 75° C.
5. stirringstirred for 10 minutes
6. temperatureThe reaction mixture was cooled to 20° C.
7. stirringthe solution was stirred in an ice water bath for 1 hour
8. customthe organic layer was separated
9. washThe organic layer was washed with saturated aqueous sodium bicarbonate solution and brine
10. dry with materialdried over magnesium sulfate
11. customThe solvent was evaporated
12. customthe residue was purified by preparative thin-layer chromatography (chloroform-methanol=10:1)