反应 #65038

反应方程式

11-Bromoundecanol

piperidine

piperidine hydrobromide

→

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

收率 96.3%

反应条件

后处理

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

实验过程

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.

来源