反应详情

A mixture of 2.30 g of compound G, 8.20 g of ammonium acetate and 8.43 g of ferric chloride hexahydrate in 50 cc of acetic acid was heated under reflux for 7 hours. After cooling, the insoluble materials were removed by filtration through Celite and the filtrate was distilled to remove the solvent. The residue was adjusted to pH 8 with an aqueous sodium bicarbonate solution, and extracted three times with ethyl acetate. The combined organic layer was washed with a saturated aqueous sodium chloride solution and dried over magnesium sulfate. The solvent was distilled off and the crude product thus obtained was purified by a silica gel column chromatography (eluent: ethyl acetate/hexane=1/5) to obtain 1.98 g of compound H. Yield: 92.1%.

1. temperaturewas heated
2. temperatureunder reflux for 7 hours
3. temperatureAfter cooling
4. customthe insoluble materials were removed by filtration through Celite
5. distillationthe filtrate was distilled
6. customto remove the solvent
7. extractionextracted three times with ethyl acetate
8. washThe combined organic layer was washed with a saturated aqueous sodium chloride solution
9. dry with materialdried over magnesium sulfate
10. distillationThe solvent was distilled off
11. customthe crude product thus obtained
12. customwas purified by a silica gel column chromatography (eluent: ethyl acetate/hexane=1/5)