4-Methoxy-1-naphthol → 4,4'-Dimethoxy[2,2'-binaphthalene]-1,1'-diol

HRID 5295

反応式

HRID 5295 の反応式
COC1C2C(=CC=CC=2)C(O)=CC=1.[CH3:14][O:15][C:16]1[C:39]2[C:34](=[CH:35][CH:36]=[CH:37][CH:38]=2)[C:32](=[O:33])/[C:18](=[C:19]2\[CH:20]=[C:21]([O:30][CH3:31])[C:22]3[C:27]([C:28]\2=[O:29])=[CH:26][CH:25]=[CH:24][CH:23]=3)/[CH:17]=1>[Ag]=O.C(Cl)(Cl)Cl>[CH3:31][O:30][C:21]1[C:22]2[C:27](=[CH:26][CH:25]=[CH:24][CH:23]=2)[C:28]([OH:29])=[C:19]([C:18]2[CH:17]=[C:16]([O:15][CH3:14])[C:39]3[C:34]([C:32]=2[OH:33])=[CH:35][CH:36]=[CH:37][CH:38]=3)[CH:20]=1

参加物

5

反応物 2

HCID 665424-Methoxy-1-naphtholHCID 53788141(2H)-Naphthalenone, 4-methoxy-2-(4-methoxy-1-oxo-2(1H)-naphthalenylidene)-

生成物 1

HCID 132842994,4'-Dimethoxy[2,2'-binaphthalene]-1,1'-diol

試薬・触媒・溶媒 2

HCID 92152Silver(II) oxide触媒HCID 6212Chloroform溶媒

実験手順

Under an atmosphere of nitrogen, a mixture of 5.0 g of 4-methoxy-1-naphthol and 50 mL chloroform was mechanically stirred with 10.0 g silver oxide until the conversion to Russig's Blue was complete. The unreacted silver oxide was filtered and washed with chloroform. The filtrate and chloroform washings were combined and stirred with 4.9 g of 4-methoxy-1-naphthol until the solution turned gray. The solution was then concentrated to 50 mL and the resulting precipitate was filtered, washed with chloroform and dried to yield 3.18 g of 1,1'-dimethoxy-3,3'-binaphthyl-4,4'-diol as a light gray solid. The structure was confirmed by NMR.

後処理

  1. filtrationThe unreacted silver oxide was filtered
  2. washwashed with chloroform
  3. concentrationThe solution was then concentrated to 50 mL
  4. filtrationthe resulting precipitate was filtered
  5. washwashed with chloroform
  6. customdried

出典と根拠

ORDレコード
ord-c2d3f9dc48864913be85c1333e2753ce
出典データセット
uspto-grants-1993_09
特許番号
US05244771

関連ノート

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