Piperidine → 11-(Piperidin-1-yl)undecan-1-ol

HRID 1886001노트

반응식

HRID 1886001 반응식
Br[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH2:10][CH2:11][CH2:12][OH:13].[NH:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1.Br.N1CCCCC1>>[OH:13][CH2:12][CH2:11][CH2:10][CH2:9][CH2:8][CH2:7][CH2:6][CH2:5][CH2:4][CH2:3][CH2:2][N:14]1[CH2:19][CH2:18][CH2:17][CH2:16][CH2:15]1

참가 물질

4

반응물 3

HCID 8082PiperidineHCID 7416311-Bromo-1-undecanolHCID 203244Piperidine, hydrobromide (1:1)

생성물 1

HCID 312228311-(Piperidin-1-yl)undecan-1-ol수율 96.3%

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.

후처리

  1. temperatureat reflux temperature for 18 hours
  2. customwas removed by filtration
  3. customThe excess piperidine is removed by simple distillation
  4. customthe resultant solid residue is recrystallized from ethanol and water
  5. customAfter drying

출처 및 근거

ORD 기록
ord-41723e7074b44283811eb5dd0fb97725
출처 데이터셋
uspto-grants-1992_09
특허 번호
US05149524

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