反応 #65038

反応方程式

11-Bromoundecanol

piperidine

piperidine hydrobromide

→

1-hydroxy-11-(N-piperidyl)undecane

収率 96.3%

反応条件

後処理

1. 1
   温度at reflux temperature for 18 hours
2. 2
   その他was removed by filtration
3. 3
   その他The excess piperidine is removed by simple distillation
4. 4
   その他the resultant solid residue is recrystallized from ethanol and water
5. 5
   その他After drying

実験手順

11-Bromoundecanol (11.00 g., 43.79 mmole) was dissolved in 100 ml. of piperidine and heated at reflux temperature for 18 hours. The reaction mixture was allowed to cool and most of the precipitated piperidine hydrobromide was removed by filtration. The excess piperidine is removed by simple distillation and the resultant solid residue is recrystallized from ethanol and water. After drying, 10.78 g. (96.3% yield) of 1-hydroxy-11-(N-piperidyl)undecane was obtained. m.p. 62°-65° C., 1H-NMR (200 MHz, CDCl3) δ=1.2-1.7 ppm, m, 24H; 2.10, broad s, 1H; 2.20-2.45, m, 6H; 3.63, t, 2H.

出典