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

HRID 654787
ノート
印刷プレビュー

反応式

HRID 654787 の反応式
[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
参加物実験手順後処理出典と根拠反応ノート

参加物

6

反応物 4

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

生成物 1

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

試薬・触媒・溶媒 1

HCID 31275
1,4-Dioxane
溶媒

実験手順

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).

後処理

  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)

出典と根拠

ORDレコード
ord-54574f63f4534a73b2a6c04759e8bd39
出典データセット
uspto-grants-1992_07
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05134142

反応ノート

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