반응 #1407

반응 방정식

3-aminopyrrolidine

pivalaldehyde

→

3-(2,2-dimethylpropylideneamino)-pyrrolidine

수율 74.0%

용매

toluene

toluene

반응 조건

후처리

1. 1
   workup.ADDITIONare added dropwise at 20° C.
2. 2
   온도while cooling in a water bath
3. 3
   기타the aqueous phase is then separated off in a separating funnel (4.6 ml)
4. 4
   건조the toluene solution is dried over sodium sulphate for 1 hour
5. 5
   기타The toluene is separated off on a rotary evaporator
6. 6
   workup.DISTILLATIONthe residue is distilled

실험 절차

34.5 g (0.4 mol) of 3-aminopyrrolidine are initially introduced into 100 ml of toluene, and 34.5 g (0.3 mol) of 75% strength pivalaldehyde (preparation from Riedel-de-Haen) in 100 ml of toluene are added dropwise at 20° C., while cooling in a water bath. The mixture is subsequently stirred at room temperature for 2 hours, the aqueous phase is then separated off in a separating funnel (4.6 ml) and the toluene solution is dried over sodium sulphate for 1 hour. The toluene is separated off on a rotary evaporator and the residue is distilled using a small Vigreux column. 46.2 g of 3-(2,2-dimethylpropylideneamino)-pyrrolidine of boiling point 61° C./10 mbar are obtained with a purity, determined by gas chromatography, of 98%, corresponding to a yield of 74% and a selectivity of 99% (pivalaldehyde).

출처