反应详情

温度

85 °C

In argon atmosphere, a mixture of 16.65 g (69.9 mmol) of 9,9-dimethyl-9H-fluorene-2-ylboronic acid, 20.00 g (69.9 mmol) of 2,7-dibromonaphthalene, 4.04 g (3.50 mmol) of tetrakis(triphenylphosphine)palladium (0), 200 ml of toluene, 200 ml of dimethoxyethane, and 106 g of a 2 M sodium carbonate aqueous solution was stirred at 85° C. for 9 h and left standing overnight. The reaction mixture was added with water and stirred at room temperature for one hour. After filtration, the filtrate was extracted with toluene. The organic phase was washed with water and then with a saturated saline solution and dried over sodium sulfate, and then the toluene was removed by distillation under reduced pressure. The obtained brown oily substance was purified by silica gel chromatography to obtain 13.4 g (yield: 48%) of 2-(7-bromonaphthalene-2-yl)-9,9-dimethyl-9H-fluorene.

1. waitleft
2. waitstanding overnight
3. stirringstirred at room temperature for one hour
4. filtrationAfter filtration
5. extractionthe filtrate was extracted with toluene
6. washThe organic phase was washed with water
7. dry with materialwith a saturated saline solution and dried over sodium sulfate
8. customthe toluene was removed by distillation under reduced pressure
9. customThe obtained brown oily substance was purified by silica gel chromatography