반응 #48582

반응 방정식

t-butylamine

1-ethyl-1-methyl-4-oxopiperidinium iodide

sodium bicarbonate

→

1-tert-butyl-4-oxopiperidine

수율 60.9%

용매

toluene

water

반응 조건

후처리

1. 1
   온도to cool to ambient temperature
2. 2
   기타The layers were separated
3. 3
   세척the aqueous layer was washed with EtOAc
4. 4
   세척washed with brine
5. 5
   건조dried (MgSO4)
6. 6
   여과filtered

실험 절차

To a solution of t-butylamine (78.2 ml, 0.74 mol) in toluene (400 ml) was added a solution of 1-ethyl-1-methyl-4-oxopiperidinium iodide (40 g, 0.148 mol) and sodium bicarbonate (1.245 g, 0.014 mol) in water (60 ml). The reaction mixture was heated at 78° C. for 6 hours and then allowed to cool to ambient temperature. The layers were separated and the aqueous layer was washed with EtOAc. The organics were combined and washed with brine, dried (MgSO4), filtered and reduced in vacuo to yield 1-tert-butyl-4-oxopiperidine (14 g) (LC/MS: Rt 0.39, [M+H]+ 156).

출처