Chloroform → 1-Methyl-3-cyclooctylmethylaminocarbonylpiperidine

HRID 483844노트

반응식

HRID 483844 반응식
C(Cl)(Cl)Cl.Cl.[CH3:6][N:7]1[CH2:15][CH2:14][CH2:13][CH:9]([C:10]([OH:12])=O)[CH2:8]1.ClC(OCC(C)C)=O.[CH:24]1([CH2:32][NH2:33])[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]1>C(N(CC)CC)C>[CH3:6][N:7]1[CH2:15][CH2:14][CH2:13][CH:9]([C:10]([NH:33][CH2:32][CH:24]2[CH2:31][CH2:30][CH2:29][CH2:28][CH2:27][CH2:26][CH2:25]2)=[O:12])[CH2:8]1

참가 물질

6

반응물 4

HCID 6212ChloroformHCID 62365Isobutyl chloroformateHCID 78473CyclooctylmethylamineHCID 125147111-Methylpiperidine-3-carboxylic acid hydrochloride

생성물 1

HCID 200816741-Methyl-3-cyclooctylmethylaminocarbonylpiperidine수율 62%

시약·촉매·용매 1

HCID 8471Triethylamine용매

실험 절차

To 80 ml of chloroform were added 3.59 g of 1-methylnipecotic acid hydrochloride and 6.26 ml of triethylamine. Thereto was added 3.0 g of isobutyl chloroformate under ice cooling and stirring. The mixture was stirred for 30 minutes. Thereto was added 3.1 g of cyclooctylmethylamine, and the mixture was subjected to a reaction for 2 hours at room temperature. The reaction mixture was washed with an aqueous sodium hydrogen carbonate solution and with water, and dried with anhydrous sodium sulfate. The solvent was removed by evaporation. The residue was purified by a Silica gel column chromatography (dichloromethane:methanol=10:1) to obtain 3.3 g of 1-methyl-3-cyclooctylmethylaminocarbonylpiperidine.

후처리

  1. stirringThe mixture was stirred for 30 minutes
  2. customthe mixture was subjected to a reaction for 2 hours at room temperature
  3. washThe reaction mixture was washed with an aqueous sodium hydrogen carbonate solution and with water
  4. dry with materialdried with anhydrous sodium sulfate
  5. customThe solvent was removed by evaporation
  6. customThe residue was purified by a Silica gel column chromatography (dichloromethane:methanol=10:1)

출처 및 근거

ORD 기록
ord-fed3f7daeda94323b55fe02cec329d8c
출처 데이터셋
uspto-grants-1993_07
특허 번호
US05227381

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