Реакция #345984

Уравнение реакции

n-octadecyl bromide

triphenyl phosphine

→

Triphenyl-n-octadecylphosphonium bromide

Растворители

toluene

Условия реакции

Обработка

1. 1
   ДругоеThe product is precipitated from the cooled solution by the addition of about 500 ml
2. 2
   Фильтрацияof ethyl acetate and the crystals filtered from solution
3. 3
   workup.ADDITIONThese crystals, 1550 grams, are added to 890 grams of sodium 3,5-dicarbomethoxybenzenesulfonate in 3000 ml
4. 4
   Температураof water which is heated to 80°-85° C.
5. 5
   ПромывкаThe oil layer is washed twice with about 2000 ml
6. 6
   Сушкаof room-temperature water, then dried at 50° C. under nitrogen for 16 hours at a pressure less than 100 torr
7. 7
   Температураon cooling

Методика

Triphenyl-n-octadecylphosphonium bromide is prepared by refluxing n-octadecyl bromide (1000 grams) and triphenyl phosphine (787 grams) in about 1400 ml. of toluene for 16 hours at about 110° C. The product is precipitated from the cooled solution by the addition of about 500 ml. of ethyl acetate and the crystals filtered from solution. These crystals, 1550 grams, are added to 890 grams of sodium 3,5-dicarbomethoxybenzenesulfonate in 3000 ml. of water which is heated to 80°-85° C. and stirred for one hour. The oil layer is washed twice with about 2000 ml. of room-temperature water, then dried at 50° C. under nitrogen for 16 hours at a pressure less than 100 torr. The product, triphenyl-n-octadecylphosphonium 3,5-dicarbomethoxybenzenesulfonate, solidifies on cooling.

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