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Methanol → 1-(4-Fluorophenyl)-3-(methoxyacetyl)-5-[4-(methylsulfonyl)phenyl]pyrazole

HRID 654787
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인쇄 미리보기

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HRID 654787 반응식
[C:1]([C:4]1[CH:8]=[C:7]([C:9]2[CH:14]=[CH:13][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:11][CH:10]=2)[N:6]([C:19]2[CH:24]=[CH:23][C:22]([F:25])=[CH:21][CH:20]=2)[N:5]=1)(=[O:3])[CH3:2].[OH2:26].O.O.[N+]([O-])([O-])=O.[Tl+3].[N+]([O-])([O-])=O.[N+]([O-])([O-])=O.Cl(O)(=O)(=O)=O.[CH3:47]O>O1CCOCC1>[F:25][C:22]1[CH:21]=[CH:20][C:19]([N:6]2[C:7]([C:9]3[CH:10]=[CH:11][C:12]([S:15]([CH3:18])(=[O:17])=[O:16])=[CH:13][CH:14]=3)=[CH:8][C:4]([C:1](=[O:3])[CH2:2][O:26][CH3:47])=[N:5]2)=[CH:24][CH:23]=1
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

6

반응물 4

HCID 887MethanolHCID 24247Perchloric AcidHCID 11270721Nitric acid,thallium(3+) salt, trihydrate (9CI)HCID 19886267HCID 19886267, 화합물

생성물 1

HCID 198862571-(4-Fluorophenyl)-3-(methoxyacetyl)-5-[4-(methylsulfonyl)phenyl]pyrazole

시약·촉매·용매 1

HCID 31275
1,4-Dioxane
용매

실험 절차

A mixture of 3-acetyl-1-(4-fluorophenyl)-5-[4-(methylsulfonyl)phenyl]pyrazole (1.1 g), thallium (III) nitrate trihydrate (1.6 g) and perchloric acid (70%; 3.3 ml) in methanol (16 ml) and dioxane (8 ml) was stirred at ambient temperature overnight. The insoluble was filtered, and the filtrate was diluted with chloroform, washed with water, dried and concentrated. The residue (1.6 g) was purified by column chromatography on silica gel (100 g) eluting with a mixture of toluene and ethyl acetate (2:1) to give pale brown crystals of 1-(4-fluorophenyl)-3-(methoxyacetyl)-5-[4-(methylsulfonyl)phenyl]pyrazole (0.13 g).

후처리

  1. filtrationThe insoluble was filtered
  2. additionthe filtrate was diluted with chloroform
  3. washwashed with water
  4. customdried
  5. concentrationconcentrated
  6. customThe residue (1.6 g) was purified by column chromatography on silica gel (100 g)
  7. washeluting with a mixture of toluene and ethyl acetate (2:1)

출처 및 근거

ORD 기록
ord-54574f63f4534a73b2a6c04759e8bd39
출처 데이터셋
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05134142

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