反应详情

温度

140 °C

2,4,6-Trimethylbenzenesulfonic acid 8-acetyl-3-(4-chlorophenyl)-2-isopropyl-4oxo-4H-chromen-7-yl ester (470 mg, 0.87 mmol), ammonium acetate (339 mg, 4.4 mmol) and magnesium sulfate (530 mg, 4.4 mmol) are dissolved/suspended in toluene (7 ml) and ethanol (7 ml) in a 20 ml capacity microwave tube. Hydrazine hydrate (0.136 ml, 4.4 mmol) is added, the tube is sealed, and the mixture is heated at 140° C. under microwave irradiation for 2 h. The reaction mixture is then poured into water (20 ml) and extracted with ethyl acetate (3×20 ml). The ethyl acetate extracts are combined, washed with saturated brine (50 ml), dried (MgSO4), filtered and evaporated to give a light brown solid. This is absorbed onto silica gel and purified by chromatography on silica gel using n-hexane/ethyl acetate (0-50% ethyl acetate) as eluant to give the product as a colourless solid.

1. customthe tube is sealed
2. extractionextracted with ethyl acetate (3×20 ml)
3. washwashed with saturated brine (50 ml)
4. dry with materialdried (MgSO4)
5. filtrationfiltered
6. customevaporated
7. customto give a light brown solid
8. customThis is absorbed onto silica gel
9. custompurified by chromatography on silica gel