alpha-(1-Methylpyrazol-5-yl)-2,3-dichloro-4,5-dimethoxybenzylalcohol → (1-Methyl-4-chloropyrazol-5-yl)-(2,3-dichloro-4,5-dimethoxyphenyl)-methanone

HRID 1074187

反応式

HRID 1074187 の反応式
[Cl:1][O-].[Na+].[CH3:4][N:5]1[C:9]([CH:10]([OH:23])[C:11]2[CH:16]=[C:15]([O:17][CH3:18])[C:14]([O:19][CH3:20])=[C:13]([Cl:21])[C:12]=2[Cl:22])=[CH:8][CH:7]=[N:6]1>C(O)(=O)C>[CH3:4][N:5]1[C:9]([C:10]([C:11]2[CH:16]=[C:15]([O:17][CH3:18])[C:14]([O:19][CH3:20])=[C:13]([Cl:21])[C:12]=2[Cl:22])=[O:23])=[C:8]([Cl:1])[CH:7]=[N:6]1

参加物

4

反応物 2

HCID 14748635alpha-(1-Methylpyrazol-5-yl)-2,3-dichloro-4,5-dimethoxybenzylalcoholHCID 23665760Sodium Hypochlorite

生成物 1

HCID 14748633(1-Methyl-4-chloropyrazol-5-yl)-(2,3-dichloro-4,5-dimethoxyphenyl)-methanone

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

実験手順

19.3 g of an aqueous 10% sodium hypochlorite solution are added to a solution of 3.9 g of α-(1-methylpyrazol-5-yl)-2,3-dichloro-4,5-dimethoxybenzylalcohol in acetic acid and the mixture is stirred at room temperature for 2 hours. The reaction mixture is concentrated to remove acetic acid, and ethyl acetate is added to the residue. The organic layer is separated, washed with water, dried and evaporated to remove solvent. The residue is purified by silica gel column chromatography to give 2.1 g of (1-methyl-4-chloropyrazol-5-yl)-(2,3-dichloro-4,5-dimethoxyphenyl)-methanone.

後処理

  1. concentrationThe reaction mixture is concentrated
  2. customto remove acetic acid, and ethyl acetate
  3. additionis added to the residue
  4. customThe organic layer is separated
  5. washwashed with water
  6. customdried
  7. customevaporated
  8. customto remove solvent
  9. customThe residue is purified by silica gel column chromatography

出典と根拠

ORDレコード
ord-39634b30ff004d2190ff7dc883dbc121
出典データセット
uspto-grants-1990_11
特許番号
US04973600

関連ノート

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