反应详情

温度

35 °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 5 gms (0.0164 mole) of tri-p-tolyl phosphine and 25 gms of toluene. The slurry is heated to 35° C. then 4.3 gms (0.0199 mole) of 3,5-dinitrobenzyl chloride is added. This reaction mass is heated to 60° C. and maintained at that temperature for 3 hours, then heated to 80° C. and maintained at that temperature for 2 hours, then cooled to 60° C. and maintained at that temperature for 16 hours, then cooed to 26° C. and filtered. The salt is washed with 3 gms of toluene and 3 gms of ethyl acetate and then vacuum dried. There is obtained 3.5 gms of catalyst which has a melting point of >250° C. and a chemical shift of 23.8 ppm (phosphoric acid reference).

1. customInto a 50 milliliter glass reactor equipped with a thermometer
2. temperatureThis reaction mass is heated to 60° C.
3. temperaturemaintained at that temperature for 3 hours
4. temperatureheated to 80° C.
5. temperaturemaintained at that temperature for 2 hours
6. temperaturecooled to 60° C.
7. temperaturemaintained at that temperature for 16 hours
8. customcooed to 26° C.
9. filtrationfiltered
10. washThe salt is washed with 3 gms of toluene and 3 gms of ethyl acetate
11. customvacuum dried
12. customThere is obtained 3.5 gms of catalyst which