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Hydrogen Bromide → 1,2-Benzenediol, 4-[1-(2-phenylethyl)-3-piperidinyl]-

HRID 616036
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반응식

HRID 616036 반응식
[C:1]1([CH2:7][CH2:8][N:9]2[CH2:14][CH2:13][CH2:12][CH:11]([C:15]3[CH:20]=[CH:19][C:18]([O:21]C)=[C:17]([O:23]C)[CH:16]=3)[CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Br>>[C:1]1([CH2:7][CH2:8][N:9]2[CH2:14][CH2:13][CH2:12][CH:11]([C:15]3[CH:20]=[CH:19][C:18]([OH:21])=[C:17]([OH:23])[CH:16]=3)[CH2:10]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 260Hydrogen BromideHCID 203708433-(3,4-Dimethoxyphenyl)-1-(2-phenylethyl)piperidine

생성물 1

HCID 64543281,2-Benzenediol, 4-[1-(2-phenylethyl)-3-piperidinyl]-수율 88.5%

실험 절차

A mixture of 3.3 g of N-(β-phenylethyl)-3-(3',4'-dimethoxyphenyl)-piperidine and 33 ml of 66% hydrobromic acid was refluxed for an hour and was then distilled to dryness under reduced pressure. The residue was taken up in a water-methylene chloride mixture and was made alkaline with an aqueous solution saturated with sodium bicarbonate. The organic phase was decanted and the aqueous phase was extracted with methylene chloride. The combined organic phases were washed with water, dried over magnesium sulfate and distilled to dryness under reduced pressure to obtain 2.67 g of N-(β-phenylethyl)-3-(3',4'-dihydroxyphenyl)-piperidine.

후처리

  1. temperaturewas refluxed for an hour
  • distillationwas then distilled to dryness under reduced pressure
  • customThe organic phase was decanted
  • extractionthe aqueous phase was extracted with methylene chloride
  • washThe combined organic phases were washed with water
  • dry with materialdried over magnesium sulfate
  • distillationdistilled to dryness under reduced pressure
  • 출처 및 근거

    ORD 기록
    ord-87a10f51aed242c8b13e038c9760f7e9
    출처 데이터셋
    uspto-grants-1978_02
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US04072685

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