反应详情

温度

30 °C

Into a 50 milliliter glass reactor equipped with a thermometer connected to a temperature controller, a heating mantle, a condenser and a magnetic stirring bar, is charged 15 gms (0.0473 mole) of tri-p-tolyl phosphine and 40 gms of xylene. The slurry is heated to 30° C., then 7 gms (0.0642 mole) of ethyl bromide is added. This reaction mass is heated to 45° C. in 1.17 hours and maintained for 21.4 hours, then cooled to 65° C. and maintained for 2.47 hours, then heated to 90° C., then maintained for 2.42 hours at that temperature, then cooled to 25° C. Then 1.5 gm (0.0138 mole) of ethyl bromide is added and maintained at 25C for 0.75 hour, then heated to 45° C. and maintained at that temperature for 16.58 hours, then heated to 70° C. and maintained at that temperature for 1.5, then cooled to 48° C. and the resulting phosphonium salt collected by filtration. After vacuum drying, there is obtained 12.8 gms of catalyst which has a melting point of 213°-220° C. and a chemical shift of 24.6 ppm (phosphoric acid reference).

1. customInto a 50 milliliter glass reactor equipped with a thermometer
2. temperatureThis reaction mass is heated to 45° C. in 1.17 hours
3. temperaturemaintained for 21.4 hours
4. temperaturecooled to 65° C.
5. temperaturemaintained for 2.47 hours
6. temperatureheated to 90° C.
7. temperaturemaintained for 2.42 hours at that temperature
8. temperaturecooled to 25° C
9. temperatureheated to 45° C.
10. temperaturemaintained at that temperature for 16.58 hours
11. temperatureheated to 70° C.
12. temperaturemaintained at that temperature for 1.5
13. temperaturecooled to 48° C.
14. filtrationthe resulting phosphonium salt collected by filtration
15. customAfter vacuum drying
16. customthere is obtained 12.8 gms of catalyst which