反应详情

Bromine (0.52 mL, 10.2 mmol) was added dropwise to a chloroform (30 mL) solution of 4-(1-methylpiperidin-4-ylidene)-9,10-dihydro-4H-3-thiabenzo[f]azulene (3.0 g, 10.2 mmol) at 0° C. The mixture was stirred at room temperature for 2 days, and a saturated aqueous sodium bicarbonate solution was then added thereto to allow separation of an organic layer. The organic layer was washed with a saturated sodium chloride solution, and then dried over anhydrous sodium sulfate. The solvents were distilled off under a reduced pressure, and the residue was then purified by column chromatography (chloroform-methanol=9:1), to give 3.8 g (100%) of the captioned compound in the form of white crystals.

1. customseparation of an organic layer
2. washThe organic layer was washed 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 then purified by column chromatography (chloroform-methanol=9:1)