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Sodium sulfate decahydrate → HCID 69217738、化合物

HRID 2221972
ノート
印刷プレビュー

反応式

HRID 2221972 の反応式
[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:30]=[CH:31][C:32]=1[O:33][CH2:34][C:35]1[N:36]=[C:37]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[O:38][C:39]=1[CH3:40])[CH2:6][O:7][C:8]1[C:12](/[CH:13]=[CH:14]/[C:15](OCC)=[O:16])=[CH:11][N:10]([C:20]2[CH:25]=[CH:24][C:23]([C:26]([F:29])([F:28])[F:27])=[CH:22][CH:21]=2)[N:9]=1.[H-].C([Al+]CC(C)C)C(C)C.O.O.O.O.O.O.O.O.O.O.S([O-])([O-])(=O)=O.[Na+].[Na+]>O1CCCC1>[CH3:1][O:2][C:3]1[CH:4]=[C:5]([CH:30]=[CH:31][C:32]=1[O:33][CH2:34][C:35]1[N:36]=[C:37]([C:41]2[CH:46]=[CH:45][CH:44]=[CH:43][CH:42]=2)[O:38][C:39]=1[CH3:40])[CH2:6][O:7][C:8]1[C:12](/[CH:13]=[CH:14]/[CH2:15][OH:16])=[CH:11][N:10]([C:20]2[CH:21]=[CH:22][C:23]([C:26]([F:27])([F:29])[F:28])=[CH:24][CH:25]=2)[N:9]=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 21225700DiisobutylaluminumhydrideHCID 86605893ethyl (2E)-3-{3-({3-methoxy-4-[(5-methyl-2-phenyl-1,3-oxazol-4-yl)methoxy]benzyl}oxy)-1-[4-(trifluoromethyl)phenyl]-1H-pyrazol-4-yl}-2-propenoate

生成物 1

HCID 69217738HCID 69217738、化合物

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran
溶媒

実験手順

To a solution of ethyl (2E)-3-{3-({3-methoxy-4-[(5-methyl-2-phenyl-1,3-oxazol-4-yl)methoxy]benzyl}oxy)-1-[4-(trifluoromethyl)phenyl]-1H-pyrazol-4-yl}-2-propenoate (0.507 g) in tetrahydrofuran (50 mL) was added diisobutylaluminum hydride (0.95 M hexane solution, 7.0 mL) at room temperature, and the mixture was stirred at room temperature for 1 hr. Sodium sulfate decahydrate (2.14 g) was added to the reaction mixture, and the mixture was further stirred for 2 hrs. After removing the precipitate by filtration, the filtrate was concentrated. The residue was subjected to silica gel column chromatography to give (2E)-3-{3-({3-methoxy-4-[(5-methyl-2-phenyl-1,3-oxazol-4-yl)methoxy]benzyl}oxy)-1-[4-(trifluoromethyl)phenyl]-1H-pyrazol-4-yl}-2-propen-1-ol as colorless crystals from a fraction eluted with tetrahydrofuran-hexane (1:1, v/v). Recrystallization from ethyl acetate-hexane gave colorless powder (0.300 g, yield 63%). melting point: 118-119° C.

後処理

  1. stirringthe mixture was further stirred for 2 hrs
  2. customAfter removing the precipitate
  3. filtrationby filtration
  4. concentrationthe filtrate was concentrated

出典と根拠

ORDレコード
ord-c2e04c656eb648119b1d5a980e989831
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実験手順後処理出典と根拠反応ノート