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

HRID 2221697
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HRID 2221697 반응식
[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
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참가 물질

5

반응물 3

HCID 62649Sodium sulfate decahydrateHCID 21226445Aluminium lithium hydrideHCID 23076555ethyl 3-(methoxymethoxy)-1-(2-methylphenyl)-1H-pyrazole-4-carboxylate

생성물 1

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

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

실험 절차

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%).

후처리

  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

출처 및 근거

ORD 기록
ord-7f518e1bf19445459449b27335b872a5
출처 데이터셋
uspto-grants-2008_05
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US07368578B2

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