Triethylamine → 1-(Pyridin-4-yl)piperidine-4-carboxylic acid

HRID 16699

반응식

HRID 16699 반응식
Cl.Cl[C:3]1[CH:8]=[CH:7][N:6]=[CH:5][CH:4]=1.C(N(CC)CC)C.[C:16]([O:24]CC)(=[O:23])[C:17]1[CH:22]=[CH:21][N:20]=[CH:19][CH:18]=1>C(O)C.O>[N:6]1[CH:7]=[CH:8][C:3]([N:20]2[CH2:21][CH2:22][CH:17]([C:16]([OH:24])=[O:23])[CH2:18][CH2:19]2)=[CH:4][CH:5]=1

참가 물질

6

반응물 3

HCID 8471TriethylamineHCID 15291Ethyl isonicotinateHCID 818524-Chloropyridine hydrochloride

생성물 1

HCID 12682891-(Pyridin-4-yl)piperidine-4-carboxylic acid수율 78.7%

시약·촉매·용매 2

HCID 702Ethanol용매2회HCID 962Water용매

반응 조건

온도
150 °C

실험 절차

4-Chloropyridine hydrochloride (9.55 g) and triethylamine (26.0 ml) are dissolved in ethanol (10 ml) and water (30 ml), and thereto is added ethyl isonicotinate (10.00 g). The reaction solution is then heated at 150° C. for 96 hours in a sealed tube. After allowing to cool, ethanol is added to the reaction solution and the insoluble materials are removed by filtration. The filtrate is concentrated under reduced pressure, and the resulting residue is suspended in chloroform. The precipitates are collected by filtration and recrystallized from water/N,N-dimethylformamide to give the title compound (10.34 g).

후처리

  1. temperatureto cool
  2. customthe insoluble materials are removed by filtration
  3. concentrationThe filtrate is concentrated under reduced pressure
  4. filtrationThe precipitates are collected by filtration
  5. customrecrystallized from water/N,N-dimethylformamide

출처 및 근거

ORD 기록
ord-cc361223dfd14718a49e0b82a2f7cfe8
출처 데이터셋
uspto-grants-2010_06
특허 번호
US07737161B2

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