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Hydrochloric Acid → 2-(2-{2-[2-(4-Ethylphenyl)ethyl]phenoxy}ethyl)-1-methypiperidine hydrochloride

HRID 743310
ノート
印刷プレビュー

反応式

HRID 743310 の反応式
[ClH:1].[CH2:2]([C:4]1[CH:9]=[CH:8][C:7]([CH2:10][CH2:11][C:12]2[CH:27]=[CH:26][CH:25]=[CH:24][C:13]=2[O:14][CH2:15][CH2:16][CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][N:18]2[CH3:23])=[CH:6][CH:5]=1)[CH3:3].C(OCC)(=O)C>O1CCOCC1>[ClH:1].[CH2:2]([C:4]1[CH:5]=[CH:6][C:7]([CH2:10][CH2:11][C:12]2[CH:27]=[CH:26][CH:25]=[CH:24][C:13]=2[O:14][CH2:15][CH2:16][CH:17]2[CH2:22][CH2:21][CH2:20][CH2:19][N:18]2[CH3:23])=[CH:8][CH:9]=1)[CH3:3]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 313Hydrochloric AcidHCID 8857Ethyl AcetateHCID 194238792-(2-{2-[2-(4-Ethylphenyl)ethyl]phenoxy}ethyl)-1-methylpiperidine

生成物 1

HCID 574976362-(2-{2-[2-(4-Ethylphenyl)ethyl]phenoxy}ethyl)-1-methypiperidine hydrochloride収率 82%

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

0.6 ml of a 4N solution of hydrogen chloride in dioxane was added to a solution of 0.650 g of 2-(2-{2-[2-(4-ethylphenyl)ethyl]phenoxy}ethyl)-1-methylpiperidine [prepared as described in step (a) above] in a suitable amount of ethyl acetate, and the resulting solution was concentrated by distillation under reduced pressure. The resulting oily residue was dissolved in ethyl acetate, and a small amount of 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 0.590 g (yield 82%) of the title compound as colorless crystals, melting at 101°-103° C.

後処理

  1. concentrationthe resulting solution was concentrated by distillation under reduced pressure
  2. dissolutionThe resulting oily residue was dissolved in ethyl acetate
  3. additiona small amount of diethyl 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-269cc9f8720e40b09e898e378749229a
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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