반응 #65038
ord-5196aa637c7740218f9e817e1b948708
반응 조건
상세 조건
See reaction.notes.procedure_details.
후처리
- 1온도at reflux temperature for 18 hours
- 2기타was removed by filtration
- 3기타The excess piperidine is removed by simple distillation
- 4기타the resultant solid residue is recrystallized from ethanol and water
- 5기타After drying
실험 절차
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.