Hydrogen Bromide → 1-Benzyl-3-(bromomethyl)piperidine

HRID 1681990노트

반응식

HRID 1681990 반응식
[CH2:1]([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14]O)[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.C(=O)([O-])[O-].[K+].[K+].[BrH:22]>>[CH2:1]([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14][Br:22])[CH2:9]1)[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1

참가 물질

4

반응물 3

HCID 260Hydrogen Bromide2회HCID 11430Potassium CarbonateHCID 10398044(1-Benzylpiperidin-3-yl)methanol

생성물 1

HCID 190759011-Benzyl-3-(bromomethyl)piperidine

실험 절차

55.1 g (0.268 mol) of N-benzyl-3-(hydroxymethyl)-piperidine are added to 400 ml of 48% hydrobromic acid with vigorous stirring and the mixture is refluxed for 1 hour. Then hydrogen bromide is introduced to saturation point (about 1 hour), the mixture is refluxed for another hour and left to stand overnight. It is then neutralized with solid potassium carbonate whilst cooling with ice and then extracted with methylene chloride. The organic phase is dried over magnesium sulphate and concentrated by evaporation in vacuo. Yield: 52.0 g (72.2% of theory), Rf value: 0.85 (aluminium oxide neutral, eluant: methylene chloride).

후처리

  1. temperaturethe mixture is refluxed for 1 hour
  2. temperaturethe mixture is refluxed for another hour
  3. waitleft
  4. temperaturecooling with ice
  5. extractionextracted with methylene chloride
  6. dry with materialThe organic phase is dried over magnesium sulphate
  7. concentrationconcentrated by evaporation in vacuo

출처 및 근거

ORD 기록
ord-febbf752e8ce4fce902c337609427ffc
출처 데이터셋
uspto-grants-1992_12
특허 번호
US05175157

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