反应详情

Into a one-liter 3-necked flask equipped with stirrer, condenser, addition funnel, and thermometer here was charged, 200 g of the above (3-bromopropyl)triphenylphosphonium bromide, and 650 ml ethanol. There was then added dropwise, 240 ml of diethylamine at 50° C. with stirring. After 18 hours at 65° C., the solution was concentrated to an oil and the residue was redissolved in 500 ml ethanol. The solution was again concentrated to a solid. The resulting brown solid was slurried in 500 ml of hot tetrahydrofuran and filtered. The crystal were recrystallized from tetrahydrofuran containing a small amount of ethanol to give 230 g of (3-diethylaminopropyl)triphenylphosphonium bromide hydrobromide (M.P. 239°-241° C.).

1. customInto a one-liter 3-necked flask equipped with stirrer, condenser, addition funnel
2. additionthermometer here was charged
3. additionThere was then added dropwise
4. concentrationthe solution was concentrated to an oil
5. dissolutionthe residue was redissolved in 500 ml ethanol
6. concentrationThe solution was again concentrated to a solid
7. filtrationfiltered
8. customThe crystal were recrystallized from tetrahydrofuran containing a small amount of ethanol