反应详情

温度

80 °C

To a 2 L 3-neck round bottom flask fitted with a glass stopper, rubber septum, and reflux condenser with a nitrogen inlet tube, was added 64.90 g (283 mmol) methyl 4-bromomethylbenzoate, 81.74 g (311 mmol) triphenylphosphine, and 744 mL toluene. The solution was heated at 80° C. for 5h. After cooling to room temperature, reaction vessel was placed in an ice bath. The resulting precipitate was filtered, washed with toluene, and dried in a vacuum oven to afford 126.35 g (89% (4-carbomethoxy) benzyltriphenylphosphonium bromide) as a white solid, mp.=248°-250° C. (reported in V. Sankaran and C. S. Marvel, J. Polym. Sci, Poly. Chem. Ed , 17, 3949 (1979) as 258°-260° C.): 1H NMR (CDCl3, 200 MHz) δ 3.86 (s,3H), 5.70 (d,J=15.3 Hz, 2H), 7.24 (m,4H), 7.71 (m, 15 H).

1. customTo a 2 L 3-neck round bottom flask fitted with a glass stopper, rubber septum
2. temperaturereflux condenser with a nitrogen inlet tube
3. temperatureAfter cooling to room temperature
4. customreaction vessel
5. customwas placed in an ice bath
6. filtrationThe resulting precipitate was filtered
7. washwashed with toluene
8. customdried in a vacuum oven