反应详情

温度

100 °C

There were mixed together 23.0 grams (1.0 mole) of sodium metal along with 90 cc. of xylene and 80 cc. of tetrahydrofurane and the mixture placed under a nitrogen atmosphere. There were then added over a 35 minute period 138.10 grams (1.0 mole) of diethyl phosphite using external cooling to control the reaction exotherm and maintain the temperature at 60° to 65° C. After addition was complete the mixture was heated to 100° C. and maintained there for about 1 hour until there was no more sodium. The mixture was cooled to 60° C. and there was started the addition of 64.5 grams (0.33 mole) of benzotrichloride (α,α,α-trichlorotoluene). The exothermic reaction was cooled to maintain the temperature at 60° to 65° C. during the 25 minute addition period. The mixture was heated at 70° to 75° C. for 7 hours and the sodium chloride filtered off. The product in the pot was then subjected to distillation, terminal conditions being a pot temperature of 205° C., distillate temperature 125° C. and pressure 4 mm. The solid residue in the pot was hexaethyl phenyl methane triphosphonate. This product was hydrolyzed and the hydrolysis product purified as in Example 1 to obtain phenyl methane triphosphonic acid.

1. temperatureexternal cooling
2. temperaturemaintain the temperature at 60° to 65° C
3. additionAfter addition
4. temperaturemaintained there for about 1 hour until there
5. temperatureThe mixture was cooled to 60° C.
6. customThe exothermic reaction
7. temperaturewas cooled
8. temperatureto maintain the temperature at 60° to 65° C.
9. additionduring the 25 minute addition period
10. temperatureThe mixture was heated at 70° to 75° C. for 7 hours
11. filtrationthe sodium chloride filtered off
12. distillationThe product in the pot was then subjected to distillation, terminal conditions
13. customa pot temperature of 205° C., distillate temperature 125° C. and pressure 4 mm
14. customthe hydrolysis product purified as in Example 1