反应详情

温度

32 °C

Into a 1 liter glass reactor equipped with a thermometer connected to a temperature controller, a heating mantle, a condenser and a magnetic stirring bar, are charged 250 gms (0.822 mole) of tri-p-tolylphosphine and 600 gms of xylene. The slurry is heated to 32° C., then 117 gms (1.073 mole) of ethyl bromide is added. This reaction mass is maintained at 32° C. for 1.5 hours, then heated to 45° C. and maintained at that temperature for 21 hrs, then heated to 65° C. and maintained at that temperature for 2 hours, then heated to 90° C. and maintained at that temperature for 2 hours. This mixture is cooled to 32° C., then 43.9 gms of ethyl bromide is added and mixed for 1 hour, then heated to 45° C. and maintained at that temperature for 18 hours, then cooled to 33° C. and an additional 15.7 gms of ethyl bromide is added and the temperature is maintained for 1 hour. The reaction mass is then heated to 45° C. and maintained at that temperature for 2 hours. The reaction material is then cooled to 50° C. and filtered. The solid phosphonium salt is washed with 200 gms of xylene resulting in 220 gms of clean phosphonium salt. The phosphonium salt has a melting point of 222°-224° C.

1. customInto a 1 liter glass reactor equipped with a thermometer
2. temperatureThis reaction mass is maintained at 32° C. for 1.5 hours
3. temperatureheated to 45° C.
4. temperaturemaintained at that temperature for 21 hrs
5. temperatureheated to 65° C.
6. temperaturemaintained at that temperature for 2 hours
7. temperatureheated to 90° C.
8. temperaturemaintained at that temperature for 2 hours
9. temperatureThis mixture is cooled to 32° C.
10. additionmixed for 1 hour
11. temperatureheated to 45° C.
12. temperaturemaintained at that temperature for 18 hours
13. temperaturecooled to 33° C.
14. temperaturethe temperature is maintained for 1 hour
15. temperatureThe reaction mass is then heated to 45° C.
16. temperaturemaintained at that temperature for 2 hours
17. temperatureThe reaction material is then cooled to 50° C.
18. filtrationfiltered
19. washThe solid phosphonium salt is washed with 200 gms of xylene resulting in 220 gms of clean phosphonium salt