反应详情

215 g (1.6 mole) of diethylene glycol monoethyl ether was introduced into a 1 l three-necked flask and slightly warmed by a mantle heater. Then, 135.4 g (0.5 mole) of phosphorus tribromide was slowly added dropwise over a period of 2 hours. The reaction mixture was cooled and poured into 500 cc of water. The desired oily product accumulated at the bottom was extracted with ether and the extract was washed with 100 cc of 10% sulfuric acid two times and with 10% sodium carbonate two times. After further washing with water two times, the extract was dried with potassium carbonate to remove ether, followed by distillation of the residue oil under reduced pressure. After removing the inital fraction of low boiling point, fractions having boiling point of 96° - 98° C/30 mmHg were collected. The yield of (I) was about 40%.

1. temperatureslightly warmed by a mantle heater
2. temperatureThe reaction mixture was cooled
3. extractionbottom was extracted with ether
4. washthe extract was washed with 100 cc of 10% sulfuric acid two times and with 10% sodium carbonate two times
5. washAfter further washing with water two times
6. dry with materialthe extract was dried with potassium carbonate
7. customto remove ether
8. distillationfollowed by distillation of the residue oil under reduced pressure
9. customAfter removing the inital fraction of low boiling point
10. customwere collected