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Hydrochloric Acid → 3-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl}-1-methylpiperidine hydrochloride

HRID 743269
ノート
印刷プレビュー

反応式

HRID 743269 の反応式
[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][C:12]2[CH:26]=[CH:25][CH:24]=[CH:23][C:13]=2[O:14][CH2:15][CH:16]2[CH2:21][CH2:20][CH2:19][N:18]([CH3:22])[CH2:17]2)[CH:7]=[CH:8][CH:9]=1.C(OCC)(=O)C>O1CCOCC1>[ClH:1].[CH3:2][O:3][C:4]1[CH:5]=[C:6]([CH2:10][CH2:11][C:12]2[CH:26]=[CH:25][CH:24]=[CH:23][C:13]=2[O:14][CH2:15][CH:16]2[CH2:21][CH2:20][CH2:19][N:18]([CH3:22])[CH2:17]2)[CH:7]=[CH:8][CH:9]=1
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 100885823-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl}-1-methylpiperidine

生成物 1

HCID 574976253-{2-[2-(3-Methoxyphenyl)ethyl]phenoxymethyl}-1-methylpiperidine hydrochloride

試薬・触媒・溶媒 1

HCID 312751,4-Dioxane溶媒

実験手順

0.5 ml of a 4N solution of hydrogen chloride in dioxane was added to a solution of 520 mg of 3-{2-[2-(3-methoxyphenyl)ethyl]phenoxymethyl}-1-methylpiperidine [prepared as described in step (a) above] in a suitable amount of ethyl acetate, and the resulting mixture was concentrated by distillation under reduced pressure, to produce the hydrochloride as a solid. This solid was dissolved in a small amount of methylene chloride, and then ethyl acetate was added to the resulting solution, which was then allowed to stand at room temperature. The crystals which precipitated were collected by filtration, to give 443 mg (yield 77%) of the title compound as colorless crystals, melting at 191°-193° C.

後処理

  1. concentrationthe resulting mixture was concentrated by distillation under reduced pressure

出典と根拠

ORDレコード
ord-e7d8cb4f4c394f7390d52aac95a4a302
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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