Potassium Carbonate → HCID 86757146, compound

Participants

Reaction Steps

In a 100 ml of reaction flask, 9.30g of n-dodecylamine (about 0.05 mol) (Tianjin Kelong Chemical Agent Factory, CP Grade) was added, and dissolved by adding 25 ml of dioxane under stirring, then 25 ml of anhydrous ethanol and 7.0 g anhydrous K2CO3 (ground) were added, heated to reflux, and 30 ml of an ethanol solution of 13 g (about 0.035 mol) of γ-chloropropyl tributyl phosphonium bromide (13 g of γ-chloropropyl tributyl phosphonium bromide was dissolved previously in 30 ml ethanol) was then added dropwise within 6 hrs under stirring and reflux, then again reacted for 2hrs under stirring and reflux, when the reaction was ended, the inorganic salt was filtered out while the solution was hot, and the solvent was distilled off from the filtrate, then the residue was cooled to room temperature, then 100 ml of diethyl ether was added to separate a large quantity of white solid, and filtered, the crude product was then obtained. The crude product was recrystallized from the mixed solvent of tetrahydrofuran and diethyl ether (volume ratio 1:1) for purification, the γ n-dodecylamino-propyl tributyl phosphonium bromide having the structural formula was then obtained: n-C12H25NH(CH2)3P+(C4H9)3 Br−.

Provenance & Evidence