反応 #48582

反応方程式

t-butylamine

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

sodium bicarbonate

→

1-tert-butyl-4-oxopiperidine

収率 60.9%

溶媒

toluene

water

反応条件

後処理

1. 1
   温度to cool to ambient temperature
2. 2
   その他The layers were separated
3. 3
   洗浄the aqueous layer was washed with EtOAc
4. 4
   洗浄washed with brine
5. 5
   乾燥dried (MgSO4)
6. 6
   ろ過filtered

実験手順

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).

出典