反应详情

温度

140 °C

16.97 g (49.9 mmoles) of 4,4'-bis (bromomethyl) biphenyl and 52.04 ml (299.4 mmoles) of triethyl-phosphite are placed in a 250 ml flask which has a cooler and oil heating bath. The mixture is heated to 140° C. under magnetic agitation for 5 hours. On completion the excess triethyl-phosphite is separated by distillation and the white solid residue, redissolved in 50 ml of ethanol, is evaporated to dryness under vacuum, this operation being repeated twice. The residue is dissolved in 30 ml of ethanol and poured slowly into a beaker containing water and ice. The precipitate obtained is filtered on porous septum G3, washed with iced water (1 l) and under vacuum dried in an oven at 40° C., obtaining 21.02 g of 4,4'-bis (phosphonomethyl) biphenyl acid tetra-ethyl ester with a molar yield of 92.8%.

1. temperatureheating bath
2. customOn completion the excess triethyl-phosphite is separated by distillation
3. dissolutionthe white solid residue, redissolved in 50 ml of ethanol
4. customis evaporated to dryness under vacuum
5. dissolutionThe residue is dissolved in 30 ml of ethanol
6. additionpoured slowly into a beaker
7. additioncontaining water and ice
8. customThe precipitate obtained
9. filtrationis filtered on porous septum G3
10. washwashed with iced water (1 l) and under vacuum
11. customdried in an oven at 40° C.