반응 #362600

반응 방정식

methylamine

6-(4-phenylbutoxy)-hexyl-bromide

potassium phthalimide

6-(4-phenyl-butoxy)-N-hexyl-phthalimide

→

6-(4-Phenylbutoxy)-hexylamine

용매

dichloromethane

acetone

반응 조건

후처리

1. 1
   온도After cooling
2. 2
   기타the potassium bromide precipitated
3. 3
   기타is removed by suction
4. 4
   여과filtering
5. 5
   workup.DISTILLATIONthe solvent is distilled off in vacuo
6. 6
   기타The oily residue thus obtained
7. 7
   기타The organic phase is separated off
8. 8
   추출the aqueous phase is extracted twice more with dichloromethane
9. 9
   건조The combined organic phases are dried over sodium sulphate
10. 10
    기타evaporated down in vacuo
11. 11
    workup.DISSOLUTIONThe oily residue is dissolved in ether
12. 12
    기타the solids precipitated
13. 13
    여과are filtered off
14. 14
    기타the filtrate is evaporated to dryness
15. 15
    workup.DISTILLATIONThe colorless oil remaining is distilled
16. 16
    기타Bp0.2 =143°-145° C.

실험 절차

A solution of 46.6 g (0.15 mol) of 6-(4-phenylbutoxy)-hexyl-bromide and 27.6 g (0.15 mol) of potassium phthalimide in 400 ml of acetone is refluxed for 70 hours. After cooling, the potassium bromide precipitated is removed by suction filtering and the solvent is distilled off in vacuo. The oily residue thus obtained, consisting of crude 6-(4-phenyl-butoxy)-N-hexyl-phthalimide, is stirred into 300 ml of dichloromethane and 300 ml of 40% methylamine solution overnight. The organic phase is separated off and the aqueous phase is extracted twice more with dichloromethane. The combined organic phases are dried over sodium sulphate and evaporated down in vacuo. The oily residue is dissolved in ether, the solids precipitated are filtered off and the filtrate is evaporated to dryness. The colorless oil remaining is distilled. Bp0.2 =143°-145° C.

출처