反应详情

The detailed preparation procedure is as follows: 3,6-dibromo-o-phenylene diamine (1.0 g, 3.7 mmol) was added to a solution of compound benzil (0.39 g, 1.84 mmol) in acetic acid (20 mL) at 120□, then the mixture was mixed uniformly. After refluxed for 12 hours, the fluid reactant was poured into water, and neutralized with sodium bicarbonate until neutral, then extracted with chloroform and washed with saturated brine, dried over anhydrous sodium sulfate, then it was vacuum evaporated to remove the solvent, and the resulting crude product was purified by column chromatography to give a white solid, and then it was purified by recrystallization from chloroform/n-hexane to give a white solid powder. The test result is: MS (EI) m/z: 440(M+).

1. customThe detailed preparation procedure
2. additionthe mixture was mixed uniformly
3. temperatureAfter refluxed for 12 hours
4. extractionthen extracted with chloroform
5. washwashed with saturated brine
6. dry with materialdried over anhydrous sodium sulfate
7. customevaporated
8. customto remove the solvent
9. customthe resulting crude product was purified by column chromatography
10. customto give a white solid
11. customit was purified by recrystallization from chloroform/n-hexane
12. customto give a white solid powder
13. customThe test result