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Sodium sulfate decahydrate → [3-({6-[(5-methyl-2-phenyl-1,3-oxazol-4-yl)methoxy]-3-phenyl-1-benzofuran-2-yl}methoxy)-1-phenyl-1H-pyrazol-4-yl]methanol

HRID 2221778
ノート
印刷プレビュー

反応式

HRID 2221778 の反応式
[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:12]=[CH:11][CH:10]=[CH:9][CH:8]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:47]=[CH:46][C:18]2[C:19]([C:40]3[CH:45]=[CH:44][CH:43]=[CH:42][CH:41]=3)=[C:20]([CH2:22][O:23][C:24]3[C:28]([C:29](OCC)=[O:30])=[CH:27][N:26]([C:34]4[CH:39]=[CH:38][CH:37]=[CH:36][CH:35]=4)[N:25]=3)[O:21][C:17]=2[CH:16]=1.[H-].[Al+3].[Li+].[H-].[H-].[H-].O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1.C(OCC)(=O)C>[CH3:1][C:2]1[O:6][C:5]([C:7]2[CH:8]=[CH:9][CH:10]=[CH:11][CH:12]=2)=[N:4][C:3]=1[CH2:13][O:14][C:15]1[CH:47]=[CH:46][C:18]2[C:19]([C:40]3[CH:41]=[CH:42][CH:43]=[CH:44][CH:45]=3)=[C:20]([CH2:22][O:23][C:24]3[C:28]([CH2:29][OH:30])=[CH:27][N:26]([C:34]4[CH:35]=[CH:36][CH:37]=[CH:38][CH:39]=4)[N:25]=3)[O:21][C:17]=2[CH:16]=1
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

6

反応物 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 69217630ethyl 3-({6-[(5-methyl-2-phenyl-1,3-oxazol-4-yl)methoxy]-3-phenyl-1-benzofuran-2-yl}methoxy)-1-phenyl-1H-pyrazole-4-carboxylate

生成物 1

HCID 69215881[3-({6-[(5-methyl-2-phenyl-1,3-oxazol-4-yl)methoxy]-3-phenyl-1-benzofuran-2-yl}methoxy)-1-phenyl-1H-pyrazol-4-yl]methanol収率 80.4%

試薬・触媒・溶媒 2

HCID 8028Tetrahydrofuran溶媒HCID 8857Ethyl Acetate溶媒

反応条件

温度
0 °C

実験手順

To a solution of ethyl 3-({6-[(5-methyl-2-phenyl-1,3-oxazol-4-yl)methoxy]-3-phenyl-1-benzofuran-2-yl}methoxy)-1-phenyl-1H-pyrazole-4-carboxylate (0.60 g) in tetrahydrofuran (10 mL) was added lithium aluminum hydride (0.055 g) at 0° C., and the mixture was stirred at 0° C. for 1 hr. Sodium sulfate decahydrate (0.46 g) was added to the reaction mixture, and the mixture was stirred at room temperature for 30 min. The reaction mixture was diluted with ethyl acetate and the precipitate was filtered off. The filtrate was concentrated to give [3-({6-[(5-methyl-2-phenyl-1,3-oxazol-4-yl)methoxy]-3-phenyl-1-benzofuran-2-yl}methoxy)-1-phenyl-1H-pyrazol-4-yl]methanol as colorless crystals (0.45 g, yield 80%). Recrystallization from ethyl acetate-hexane gave colorless prism crystals. melting point: 118-119° C.

後処理

  1. stirringthe mixture was stirred at room temperature for 30 min
  2. filtrationthe precipitate was filtered off
  3. concentrationThe filtrate was concentrated

出典と根拠

ORDレコード
ord-69ac43988620494bb034e7e3ddfc41bf
出典データセット
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07368578B2

反応ノート

読み込み中…

このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート