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Hydrochloric Acid → 3-{2-[2-(3-Methoxyphenyl)ethyl]phenoxy}piperidine hydrochloride

HRID 743271
ノート
印刷プレビュー

反応式

HRID 743271 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([O:14][C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[CH2:21][CH2:22][C:23]2[CH:28]=[CH:27][CH:26]=[C:25]([O:29][CH3:30])[CH:24]=2)[CH2:9]1)=O)(C)(C)C.[ClH:31]>O1CCOCC1>[ClH:31].[CH3:30][O:29][C:25]1[CH:24]=[C:23]([CH2:22][CH2:21][C:16]2[CH:17]=[CH:18][CH:19]=[CH:20][C:15]=2[O:14][CH:10]2[CH2:11][CH2:12][CH2:13][NH:8][CH2:9]2)[CH:28]=[CH:27][CH:26]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

HCID 313Hydrochloric AcidHCID 105017801-t-Butoxycarbonyl-3-{2-[2-(3-methoxyphenyl)ethyl]phenoxy}piperidine

生成物 1

HCID 194239033-{2-[2-(3-Methoxyphenyl)ethyl]phenoxy}piperidine hydrochloride収率 44%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

800 mg of 1-t-butoxycarbonyl-3-{2-[2-(3-methoxyphenyl) ethyl]phenoxy}piperidine [prepared as described in step (a) above] were dissolved in 8 ml of a 4N solution of hydrogen chloride in dioxane, and the solution was allowed to stand at room temperature for 2 hours. At the end of this time, the solution was concentrated by evaporation under reduced pressure, the resulting residue was dissolved in ethyl acetate, and the resulting solution was allowed to stand at room temperature. The crystals which precipitated were collected by filtration, to give 300 mg (yield 44%) of the title compound as colorless crystals, melting at 130°-132° C.

後処理

  1. concentrationAt the end of this time, the solution was concentrated by evaporation under reduced pressure
  2. dissolutionthe resulting residue was dissolved in ethyl acetate
  3. customto stand at room temperature
  4. customThe crystals which precipitated
  5. filtrationwere collected by filtration

出典と根拠

ORDレコード
ord-1a47371cdd1c497883d1a50fcc8f6b83
出典データセット
uspto-grants-1996_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05556864

反応ノート

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