反应详情

To a solution containing 10 g (45.8 mmole) of p-chlorocarbonylmethylbenzoate dissolved in 100 ml of dichlorobenzene was added 3.0 g (15.3 mmole) of 1,2-diamino-4,5-dinitrobenzene. After heating the resulting mixture to reflux under nitrogen (frothing), it was maintained at that temperature for 2 hours. The solution was then allowed to cool in ice for one hour, and the precipitate that formed was filtered by suction, washed with benzene and air-dried. Recrystallization from tetrahydrofuran (THF)-n-propanol by distillation to a small volume in vacuo yielded 3.2 g (62%) of 2-[p-carbomethoxyphenyl]-5,6-dinitrobenzimidazole as light yellow needles, m.p. 239°-240°.

1. temperatureAfter heating the resulting mixture
2. temperatureto reflux under nitrogen (frothing)
3. temperatureit was maintained at that temperature for 2 hours
4. temperatureto cool in ice for one hour
5. customthe precipitate that formed
6. filtrationwas filtered by suction
7. washwashed with benzene
8. customair-dried
9. customRecrystallization from tetrahydrofuran (THF)-n-propanol
10. distillationby distillation to a small volume in vacuo