反应详情

A 500 ml four-necked flask with stirrer, thermometer, dropping funnel with pressure compensation and reflux condenser was charged with 300.0 g of phosphoryl chloride at 20° C. Then a vacuum of 200 mbar was applied and 45.0 g of 1,4-butanediol were added dropwise over the course of 45 minutes. Cooling in an ice-water bath kept the temperature at 20° C. A clear, colourless reaction mixture was formed. After the end of the metered addition, the pressure was lowered to about 100 mbar, and stirring was continued for 2 hours. A distillation bridge was then mounted on, and the excess of phosphoryl chloride was removed by distillation. This left 144.9 g (91%) of 1,4-butanediol bis(dichlorophosphate).

1. customA 500 ml four-necked flask with stirrer, thermometer, dropping
2. temperaturefunnel with pressure compensation and reflux condenser
3. temperatureCooling in an ice-water bath
4. customat 20° C
5. customA clear, colourless reaction mixture was formed
6. additionAfter the end of the metered addition
7. customwas removed by distillation