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Sodium sulfate decahydrate → [3-(methoxymethoxy)-1-(2-methylphenyl)-1H-pyrazol-4-yl]methanol

HRID 2221697
ノート
印刷プレビュー

反応式

HRID 2221697 の反応式
[CH3:1][O:2][CH2:3][O:4][C:5]1[C:9]([C:10](OCC)=[O:11])=[CH:8][N:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[CH3:21])[N:6]=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>[CH3:1][O:2][CH2:3][O:4][C:5]1[C:9]([CH2:10][OH:11])=[CH:8][N:7]([C:15]2[CH:20]=[CH:19][CH:18]=[CH:17][C:16]=2[CH3:21])[N:6]=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 21226445Aluminium lithium hydrideHCID 23076555ethyl 3-(methoxymethoxy)-1-(2-methylphenyl)-1H-pyrazole-4-carboxylate

生成物 1

HCID 69217086[3-(methoxymethoxy)-1-(2-methylphenyl)-1H-pyrazol-4-yl]methanol収率 90%

試薬・触媒・溶媒 1

HCID 8028Tetrahydrofuran溶媒

実験手順

To a solution of ethyl 3-(methoxymethoxy)-1-(2-methylphenyl)-1H-pyrazole-4-carboxylate (2.39 g) in tetrahydrofuran (60 mL) was added lithium aluminum hydride (0.323 g) at 0° C. and the mixture was stirred at room temperature for 16 hrs. Sodium sulfate decahydrate (2.78 g) was added to the reaction mixture and the mixture was stirred at room temperature for 1 hr. After removing the precipitate by filtration, and the filtrate was concentrated. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate-hexane (1:1-4:1, v/v) to give [3-(methoxymethoxy)-1-(2-methylphenyl)-1H-pyrazol-4-yl]methanol as a pale-yellow oil (1.84 g, yield 90%).

後処理

  1. stirringthe mixture was stirred at room temperature for 1 hr
  2. customAfter removing the precipitate
  3. filtrationby filtration
  4. concentrationthe filtrate was concentrated
  5. washeluted with ethyl acetate-hexane (1:1-4:1

出典と根拠

ORDレコード
ord-7f518e1bf19445459449b27335b872a5
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

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