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Dimethylamine → HCID 178463128、化合物

HRID 399940
ノート
印刷プレビュー

反応式

HRID 399940 の反応式
[CH2:1]([N:3]1[C:7]([OH:8])=[C:6]([C:9](=[O:22])[C:10]2[CH:15]=[CH:14][C:13]([S:16]([CH3:19])(=[O:18])=[O:17])=[C:12](Cl)[C:11]=2[Cl:21])[CH:5]=[N:4]1)[CH3:2].[CH3:23][NH:24][CH3:25]>>[CH2:1]([N:3]1[C:7]([OH:8])=[C:6]([C:9](=[O:22])[C:10]2[CH:15]=[CH:14][C:13]([S:16]([CH3:19])(=[O:18])=[O:17])=[C:12]([N:24]([CH3:25])[CH3:23])[C:11]=2[Cl:21])[CH:5]=[N:4]1)[CH3:2]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

3

反応物 2

HCID 674DimethylamineHCID 178463117HCID 178463117、化合物

生成物 1

HCID 178463128HCID 178463128、化合物

反応条件

温度
110 °C

実験手順

A mixture of 0.60 g (1.7 mmol) of 1-ethyl-4-(2,3-dichloro-4-methylsulfonylbenzoyl)-5-hydroxypyrazole and 8 mL of 40 percent aqueous dimethylamine was placed in a pressure reactor and heated at 110° C. for 24 hours. It was then allowed to cool and was concentrated by evaporation under reduced pressure. The residue was dissolved in dichloromethane and the solution obtained was washed with 1N aqueous hydrochloric acid, dried over sodium sulfate, and concentrated by evaporation under reduced pressure to obtain about 0.50 g of a yellow foam. This was crystallized from ethanol to obtain, after drying for 24 hours at 50° C., 0.17 g of the title compound as an off-white solid melting at 227°-228° C. with decomposition.

後処理

  • customwas placed in a pressure reactor
  • temperatureto cool
  • concentrationwas concentrated by evaporation under reduced pressure
  • dissolutionThe residue was dissolved in dichloromethane
  • customthe solution obtained
  • washwas washed with 1N aqueous hydrochloric acid
  • dry with materialdried over sodium sulfate
  • concentrationconcentrated by evaporation under reduced pressure
  • 出典と根拠

    ORDレコード
    ord-eeac39b043c94603b833bbf96f10c563
    出典データセット
    uspto-grants-1998_10
    DOI
    10.6084/m9.figshare.5104873.v1
    特許番号
    US05824802

    反応ノート

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    このページの内容参加物反応条件実験手順後処理出典と根拠反応ノート