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

HRID 743267
ノート
印刷プレビュー

反応式

HRID 743267 の反応式
C(OC([N:8]1[CH2:13][CH2:12][CH2:11][CH:10]([CH2:14][O:15][C:16]2[CH:21]=[CH:20][CH:19]=[CH:18][C:17]=2[CH2:22][CH2:23][C:24]2[CH:29]=[CH:28][CH:27]=[C:26]([O:30][CH3:31])[CH:25]=2)[CH2:9]1)=O)(C)(C)C.[ClH:32]>O1CCOCC1>[ClH:32].[CH3:31][O:30][C:26]1[CH:25]=[C:24]([CH2:23][CH2:22][C:17]2[CH:18]=[CH:19][CH:20]=[CH:21][C:16]=2[O:15][CH2:14][CH:10]2[CH2:11][CH2:12][CH2:13][NH:8][CH2:9]2)[CH:29]=[CH:28][CH:27]=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 117966521-t-Butoxycarbonyl-3-{2-[2-(3-methoxyphenyl)ethyl]phenoxymethyl}piperidine

生成物 1

HCID 574976243-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl]piperidine hydrochloride収率 76%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

240 mg of 1-t-butoxycarbonyl-3-{2-[2-(3-methoxyphenyl)ethyl]phenoxymethyl}piperidine [prepared as described in step (a) above] were dissolved in 4 ml of a 4N solution of hydrogen chloride in dioxane. The solution was allowed to stand at room temperature for 3 hours, after which it was concentrated by evaporation under reduced pressure. The resulting residue was dissolved in ethyl acetate, and the solution was allowed to stand at room temperature. The crystals which precipitated were collected by filtration, to give 183 mg (yield 76%) of the title compound as colorless crystals, melting at 155°-157° C.

後処理

  1. concentrationafter which it 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-4d5f4a387e254360931320719867b9c7
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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