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Aluminium lithium hydride → HCID 22909714, 화합물

HRID 1078646
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HRID 1078646 반응식
C([O:3][C:4]([C:6]1[CH:11]=[CH:10][C:9]([N:12]2[C:16]([C:17]3[CH:22]=[CH:21][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:19][CH:18]=3)=[CH:15][C:14]([C:27]([F:30])([F:29])[F:28])=[N:13]2)=[CH:8][CH:7]=1)=O)C.[H-].[Al+3].[Li+].[H-].[H-].[H-]>O1CCCC1>[OH:3][CH2:4][C:6]1[CH:11]=[CH:10][C:9]([N:12]2[C:16]([C:17]3[CH:18]=[CH:19][C:20]([S:23]([CH3:26])(=[O:25])=[O:24])=[CH:21][CH:22]=3)=[CH:15][C:14]([C:27]([F:28])([F:29])[F:30])=[N:13]2)=[CH:8][CH:7]=1
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

4

반응물 2

HCID 21226445Aluminium lithium hydrideHCID 22909667HCID 22909667, 화합물

생성물 1

HCID 22909714HCID 22909714, 화합물수율 59.9%

시약·촉매·용매 1

HCID 8028Tetrahydrofuran용매

반응 조건

온도
55 °C

실험 절차

A mixture of 1-[4-(ethoxycarbonyl)phenyl]-5-[4-(methylsulfonyl)phenyl]-3-(trifluoromethyl)pyrazole (2.4 g) and lithium aluminum hydride (0.25 g) in tetrahydrofuran (20 ml) was stirred at 55° C. for 2 hours. The reaction was quenched with methanol and water, and the mixture was filtered. The filtrate was concentrated and the residue was dissolved in a mixture of ethyl acetate and tetrahydrofuran. The solution was washed with water, dried, and evaporated. The residue was purified by column chromatography on silica gel eluting with a mixture of chloroform and methanol (20:1).to give a white powder of 1-[4-(hydroxymethyl)phenyl]-5-[4-(methylsulfonyl)phenyl]-3-(trifluoromethyl)pyrazole (1.3 g).

후처리

  1. customThe reaction was quenched with methanol and water
  2. filtrationthe mixture was filtered
  3. concentrationThe filtrate was concentrated
  4. dissolutionthe residue was dissolved in a mixture of ethyl acetate and tetrahydrofuran
  5. washThe solution was washed with water
  6. customdried
  7. customevaporated
  8. customThe residue was purified by column chromatography on silica gel eluting with a mixture of chloroform and methanol (20:1).to

출처 및 근거

ORD 기록
ord-dd227248604645759fa94dd9e9a426af
출처 데이터셋
uspto-grants-1996_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05550147

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