反应详情

Tri-n-octyl-n-butylphosphonium bromide is prepared by slowing dripping tri-(n-octyl)phosphine (740 grams) into refluxing 1-bromobutane (500 grams) in a nitrogen atmosphere. Reflux is continued one hour after final addition then the solution is cooled with stirring for about 18 hours, followed by vacuum removal of excess 1-bromobutane at 60° C. This product, 1210 grams from two successive preparations, is added to 880 grams of sodium 3,5-dicarbomethoxybenzenesulfonate in 2500 ml. of water and stirred for at least one hour at 85° C. then the heat is removed and the oil-in-water mixture is stirred for about 18 hours. The oil layer is separated from the water, rinsed with 1000 ml. of water and dried at about 80° C. at a pressure less than 2 torr for 18 hours. This product, an oil, is tri-n-octyl-n-butylphosphonium 3,5-dicarbomethoxybenzenesulfonate with 4.2% phosphorus and 4.7% sulfur by analysis.

1. temperatureReflux
2. additionafter final addition
3. temperaturethe solution is cooled
4. customfollowed by vacuum removal of excess 1-bromobutane at 60° C
5. additionThis product, 1210 grams from two successive preparations, is added to 880 grams of sodium 3,5-dicarbomethoxybenzenesulfonate in 2500 ml
6. stirringof water and stirred for at least one hour at 85° C.
7. customthe heat is removed
8. stirringthe oil-in-water mixture is stirred for about 18 hours
9. customThe oil layer is separated from the water
10. washrinsed with 1000 ml
11. dry with materialof water and dried at about 80° C. at a pressure less than 2 torr for 18 hours