Sodium sulfate decahydrate → [1-[4-(2-phenyl-4-oxazolylmethoxy)benzyl]-3-(2-thienyl)-1H-pyrazol-4-yl]methanol

HRID 350026ノート

反応式

HRID 350026 の反応式
[H-].[Al+3].[Li+].[H-].[H-].[H-].[C:7]1([C:13]2[O:14][CH:15]=[C:16]([CH2:18][O:19][C:20]3[CH:41]=[CH:40][C:23]([CH2:24][N:25]4[CH:29]=[C:28]([C:30](OCC)=[O:31])[C:27]([C:35]5[S:36][CH:37]=[CH:38][CH:39]=5)=[N:26]4)=[CH:22][CH:21]=3)[N:17]=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[O:14][CH:15]=[C:16]([CH2:18][O:19][C:20]3[CH:41]=[CH:40][C:23]([CH2:24][N:25]4[CH:29]=[C:28]([CH2:30][OH:31])[C:27]([C:35]5[S:36][CH:37]=[CH:38][CH:39]=5)=[N:26]4)=[CH:22][CH:21]=3)[N:17]=2)[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=1

参加物

5

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23024977ethyl 1-[4-(2-phenyl-4-oxazolylmethoxy)benzyl]-3-(2-thienyl)-1H-pyrazole-4-carboxylate

生成物 1

HCID 69422251[1-[4-(2-phenyl-4-oxazolylmethoxy)benzyl]-3-(2-thienyl)-1H-pyrazol-4-yl]methanol収率 94%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

Lithium aluminium hydride (210 mg) was added portionwise to a solution of ethyl 1-[4-(2-phenyl-4-oxazolylmethoxy)benzyl]-3-(2-thienyl)-1H-pyrazole-4-carboxylate (2.73 g) in tetrahydrofuran (50 ml) at 0° C., which was stirred for 30 minutes. After sodium sulfate decahydrate (1.80 g) was added to the reaction mixture, and the precipitate was removed by filtration, the filtrate was concentrated. The residue was subjected to silica gel column chromatography to obtain [1-[4-(2-phenyl-4-oxazolylmethoxy)benzyl]-3-(2-thienyl)-1H-pyrazol-4-yl]methanol (2.33 g, yield: 94%) as colorless crystals from the fraction eluted with ethyl acetate-hexane (1:1, volume ratio). This was recrystallized from ethyl acetate-hexane. Melting point: 155˜156° C.

後処理

  1. customthe precipitate was removed by filtration
  2. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-7296b31de75e4660b8f1ccabf4919a88
出典データセット
uspto-grants-2007_02
特許番号
US07179823B1

反応ノート

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