反应详情

In an 100 mL three-necked RB flask equipped with a magnetic bar, a condenser and a nitrogen gas inlet, 2-bromo-6-methoxynaphthalene (7.32 g, 30 mmol), 4-methoxybenzene boronic acid (4.86 g, 32 mmol) and 1-propanol (50 mL) were mixed and stirred at room temperature for approx. 30 min. Palladium acetate (0.02 g, 0.09 mmol), triphenylphosphine (0.07 g, 0.27 mmol), Na2CO3 solution (2M, 18 mL, 36 mmol) and water (10 mL) were added and the mixture was refluxed for 1.5 h. When the mixture was still hot, 30 mL of water was added and the mixture was stirred and cooled to room temperature. The resultant crystals were filtered, washed with water and recrystallized from acetone to give the DMPN title compound as colorless flakes (6.86 g, 86%). mp 194–196° C. (DSC 196° C). 1H NMR (500 MHz, CDCl3) δ 3.88 (s, 3H), 3.95 (s, 3H), 7–8 (m, 10 H). IR (KBr) ν (cm−): 3058 (Ph-H, w), 1028 (OCH3, s). Anal. Calcd for C18H16O2: C, 81.79; H, 6.10. Found: C, 81.80; H, 6.25. GC-MS (m/z) 264 (M+).

1. customIn an 100 mL three-necked RB flask equipped with a magnetic bar, a condenser and a nitrogen gas inlet
2. temperaturethe mixture was refluxed for 1.5 h
3. stirringthe mixture was stirred
4. temperaturecooled to room temperature
5. filtrationThe resultant crystals were filtered
6. washwashed with water
7. customrecrystallized from acetone