반응 #1409

반응 방정식

1-benzyl-3-benzylaminopyrrolidine

charcoal

→

3-(2,2-dimethyl-propylidene-amino)-pyrrolidine

수율 58.0%

용매

methanol

반응 조건

후처리

1. 1
   기타for 10 hours
2. 2
   여과The catalyst is filtered off
3. 3
   workup.ADDITION16.6 g (0.138 mol ) of 71% strength pivalaldehyde are added to the filtrate
4. 4
   기타rises from 20° C. to 28° C
5. 5
   workup.STIRRINGThe mixture is subsequently stirred for 30 minutes
6. 6
   기타the methanol is removed on a rotary evaporator
7. 7
   workup.DISTILLATIONthe residue is distilled

실험 절차

36.8 g (0.138 mol) of 1-benzyl-3-benzylaminopyrrolidine are hydrogenated in 160 ml of methanol over 5 g of 5% strength palladium on active charcoal at 130° C. under a hydrogen pressure of 100 bar for 10 hours. The catalyst is filtered off and 16.6 g (0.138 mol ) of 71% strength pivalaldehyde are added to the filtrate, while stirring, after which the temperature rises from 20° C. to 28° C. The mixture is subsequently stirred for 30 minutes, the methanol is removed on a rotary evaporator and the residue is distilled. 12.7 g of 3-(2,2-dimethyl-propylidene-amino)-pyrrolidine of boiling point: 61° C./10 mbar are obtained with a purity, determined by gas chromatography, of 97%, corresponding to a yield of 58% of theory.

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