rel-(2R,6S)-2,6-Dimethylpiperidine → 1-(2-(2,6-Dimethylpiperidyl)ethoxy)-4-((4-chloronaphthyloxy)methyl)benzene

HRID 1296849

反応式

HRID 1296849 の反応式
Cl[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][O:12][C:13]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16]([Cl:23])=[CH:15][CH:14]=2)=[CH:7][CH:6]=1.[CH3:24][C@H:25]1[CH2:30][CH2:29][CH2:28][C@@H:27]([CH3:31])[NH:26]1>>[CH3:24][CH:25]1[CH2:30][CH2:29][CH2:28][CH:27]([CH3:31])[N:26]1[CH2:2][CH2:3][O:4][C:5]1[CH:10]=[CH:9][C:8]([CH2:11][O:12][C:13]2[C:22]3[C:17](=[CH:18][CH:19]=[CH:20][CH:21]=3)[C:16]([Cl:23])=[CH:15][CH:14]=2)=[CH:7][CH:6]=1

参加物

3

反応物 2

HCID 641768rel-(2R,6S)-2,6-DimethylpiperidineHCID 235143952-Chloro-1-(4-((4-chloronaphthyloxy)methyl)phenoxy)ethane

生成物 1

HCID 235144091-(2-(2,6-Dimethylpiperidyl)ethoxy)-4-((4-chloronaphthyloxy)methyl)benzene収率 47.2%

実験手順

A stirred mixture of 0.4 grams (0.001 mole) of 2-chloro-1-(4-((4-chloronaphthyloxy)methyl)phenoxy)ethane and 5 mL (0.037 mole) of cis-2,6-dimethylpiperidine was heated to just below reflux for about 72 hours. After this time, the reaction mixture was analyzed by thin layer chromatography (TLC), which indicated the reaction was incomplete. The reaction mixture was concentrated under reduced pressure and subject to column chromatography on silica gel, yielding 0.2 gram of compound 106. The NMR spectrum was consistent with the proposed structure.

後処理

  1. temperaturewas heated to just
  2. temperaturebelow reflux for about 72 hours
  3. concentrationThe reaction mixture was concentrated under reduced pressure

出典と根拠

ORDレコード
ord-01e21882f70e44d7ad4b31fa479f4c53
出典データセット
uspto-grants-2007_07
特許番号
US07247756B2

関連ノート

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