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Sodium sulfate decahydrate → (5-Phenylpyridin-3-yl)methanol

HRID 349967
ノート
印刷プレビュー

反応式

HRID 349967 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([C:13]2[CH:14]=[C:15]([C:19](OCC)=[O:20])[CH:16]=[N:17][CH:18]=2)[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=1.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[C:7]1([C:13]2[CH:14]=[C:15]([CH2:19][OH:20])[CH:16]=[N:17][CH:18]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=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 62649Sodium sulfate decahydrateHCID 15530815Ethyl 5-phenylnicotinateHCID 21226445Aluminium lithium hydride

生成物 1

HCID 22254272(5-Phenylpyridin-3-yl)methanol収率 69%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium aluminium hydride (1.45 g) was added to a solution of ethyl 5-phenyl-3-pyridinecarboxylate (8.60 g) in tetrahydrofuran (100 ml) at 0° C., which was stirred at room temperature for 30 minutes. Sodium sulfate decahydrate (13.40 g) was added to the reaction mixture, which was stirred at room temperature for 30 minutes. The precipitate was removed by filtration, and the filtrate was concentrated. The resulting colorless crystals were collected by filtration to obtain 5-phenyl-3-pyridylmethanol (4.82 g, yield 69%). This was recrystallized from ethyl acetate-hexane. Melting point: 71–72° C.

後処理

  1. stirringwas stirred at room temperature for 30 minutes
  2. customThe precipitate was removed by filtration
  3. concentrationthe filtrate was concentrated
  4. filtrationThe resulting colorless crystals were collected by filtration

出典と根拠

ORDレコード
ord-9c9b549899e848bba36a68dc211598ff
出典データセット
uspto-grants-2007_02
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07179823B1

反応ノート

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