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Hydrochloric Acid → 2-(2-{2-[2-(4-Ethylphenyl)ethyl]phenoxy}-ethyl) piperidine hydrochloride

HRID 743308
ノート
印刷プレビュー

反応式

HRID 743308 の反応式
[ClH:1].C(OC([N:9]1[CH2:14][CH2:13][CH2:12][CH2:11][CH:10]1[CH2:15][CH2:16][O:17][C:18]1[CH:23]=[CH:22][CH:21]=[CH:20][C:19]=1[CH2:24][CH2:25][C:26]1[CH:31]=[CH:30][C:29]([CH2:32][CH3:33])=[CH:28][CH:27]=1)=O)(C)(C)C>O1CCOCC1>[ClH:1].[CH2:32]([C:29]1[CH:28]=[CH:27][C:26]([CH2:25][CH2:24][C:19]2[CH:20]=[CH:21][CH:22]=[CH:23][C:18]=2[O:17][CH2:16][CH2:15][CH:10]2[CH2:11][CH2:12][CH2:13][CH2:14][NH:9]2)=[CH:31][CH:30]=1)[CH3:33]
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 194238691-t-Butoxycarbonyl-2-(2-{2-[2-(4-ethylphenyl)ethyl]phenoxy}ethyl)piperidine

生成物 1

HCID 194238282-(2-{2-[2-(4-Ethylphenyl)ethyl]phenoxy}-ethyl) piperidine hydrochloride収率 88%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒2 回

実験手順

5 ml of a 4N solution of hydrogen chloride in dioxane were added to a solution of 0.91 g of 1-t-butoxycarbonyl-2-(2-{2-[2-(4-ethylphenyl)ethyl]phenoxy}ethyl)piperidine [prepared as described in step (a) above] in 5 ml of dioxane, and the resulting solution was allowed to stand at room temperature for 1 hour. At the end of this time, the mixture was concentrated by distillation under reduced pressure, and the resulting oily residue was dissolved in a small amount of ethyl acetate. Diethyl ether was added to the solution, which was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration and dried in vacuo, to give 687 mg (yield 88%) of the title compound as colorless crystals, melting at 74°-76° C.

後処理

  1. concentrationAt the end of this time, the mixture was concentrated by distillation under reduced pressure
  2. dissolutionthe resulting oily residue was dissolved in a small amount of ethyl acetate
  3. additionDiethyl ether was added to the solution, which
  4. customto stand at room temperature
  5. customThe crystals which precipitated
  6. filtrationwere collected by filtration
  7. customdried in vacuo

出典と根拠

ORDレコード
ord-75bc5785889d4156a105d41cca3402e1
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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