反应详情

Bromine (8.5 mL, 165 mmol) was added dropwise to a chloroform (300 mL) solution of 9,10-dihydro-1-thiabenzo[f]azulen-4-one (23.2 g, 108 mmol), and the mixture was stirred for 4 hours. Water was added to the reaction mixture, the product was extracted with ethyl acetate, the organic layer was then washed with a saturated aqueous sodium bicarbonate solution and with a saturated sodium chloride solution, and dried over anhydrous sodium sulfate. The solvents were distilled off under a reduced pressure, and the residue was purified by silica gel chromatography (hexane-ethyl acetate), to give 22.0 g (69%) of the captioned compound.

1. extractionthe product was extracted with ethyl acetate
2. washthe organic layer was then washed with a saturated aqueous sodium bicarbonate solution and with a saturated sodium chloride solution
3. dry with materialdried over anhydrous sodium sulfate
4. distillationThe solvents were distilled off under a reduced pressure
5. customthe residue was purified by silica gel chromatography (hexane-ethyl acetate)