반응 #214090

반응 방정식

cyclohexylamine

1,4-dichlorobutene

→

1-Cyclohexyl- 3 -pyrroline

수율 76.0%

용매

benzene

반응 조건

후처리

1. 1
   workup.ADDITIONTo the solution was added
2. 2
   온도Heat
3. 3
   온도the reactants were heated
4. 4
   온도at reflux temperature for 18 hours
5. 5
   온도The mixture was cooled to about 50° C.
6. 6
   여과filtered
7. 7
   기타to remove the hydrochloride
8. 8
   기타Carbon dioxide was bubbled into the filtrate
9. 9
   기타to precipitate excess amine carbonate which
10. 10
    기타was removed by filtration
11. 11
    기타Solvent was removed from the filtrate by distillation under reduced pressure

실험 절차

A solution of 5.19 kg (52.3 moles) of cyclohexylamine in 4.0 liters of benzene was heated to mild reflux (92° C.) and then the heating discontinued. To the solution was added, dropwise, 1,635 g (13.1 moles) of 1,4-dichlorobutene at a rate sufficient to maintain gentle reflux, 3 hours time being required. Heat was reapplied and the reactants were heated at reflux temperature for 18 hours. The mixture was cooled to about 50° C. and filtered to remove the hydrochloride. Carbon dioxide was bubbled into the filtrate to precipitate excess amine carbonate which was removed by filtration. Solvent was removed from the filtrate by distillation under reduced pressure and the reddish fluid residue slightly contaminated with benzene weighed 1,506 g (76% yield).

출처