反应详情

温度

62 °C

There were charged into the reaction vessel 23.0 grams (1.0 mole) of sodium metal along with 90 cc. of xylene and 80 cc. of tetrahydrofurane. The vessel was placed under a nitrogen blanket and 138.10 grams (1.0 mole) of diethyl phosphite added over a 35 minute period. An exothermic reaction ensued which was maintained at 62° C. by external cooling. After addition was complete the mixture was heated to 100° C. and held there until all of the sodium metal was gone. The mixture was cooled to 60° to 70° C. and 80.50 grams (0.5 mole) of benzal chloride were added gradually over a 25 minute period. An exothermic reaction ensued which was maintained at 60° to 70° C. by external cooling. The mixture was then heated for 4 hours at 70° to 75° C., cooled to 60° C. The liquid material was separated from the solid and the solid boiled 8 times with 100 cc. of benzene to extract the organic material. The eluate product was then distilled, terminal conditions being a pot temperature of 201° C., distillate temperature 125° C. and pressure 6 mm. The solid residue of 70 grams was tetraethyl phenyl methane diphosphonate. This product was hydrolyzed and the hydrolysis product purified as in Example 1 to obtain phenyl methane diphosphonic acid.

1. additionadded over a 35 minute period
2. customAn exothermic reaction
3. additionAfter addition
4. temperaturewas heated to 100° C.
5. temperatureThe mixture was cooled to 60° to 70° C.
6. customAn exothermic reaction
7. temperaturewas maintained at 60° to 70° C. by external cooling
8. temperatureThe mixture was then heated for 4 hours at 70° to 75° C.
9. temperaturecooled to 60° C
10. customThe liquid material was separated from the solid
11. extractionof benzene to extract the organic material
12. distillationThe eluate product was then distilled
13. customa pot temperature of 201° C., distillate temperature 125° C. and pressure 6 mm
14. customthe hydrolysis product purified as in Example 1