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

HRID 616036
ノート
印刷プレビュー

反応式

HRID 616036 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

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

生成物 1

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

実験手順

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.

後処理

  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
  • 出典と根拠

    ORDレコード
    ord-87a10f51aed242c8b13e038c9760f7e9
    出典データセット
    uspto-grants-1978_02
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US04072685

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