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Dimethylamine → HCID 178463128, 화합물

HRID 399940
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HRID 399940 반응식
[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]
참가 물질반응 조건실험 절차후처리출처 및 근거반응 노트

참가 물질

3

반응물 2

HCID 674DimethylamineHCID 178463117HCID 178463117, 화합물

생성물 1

HCID 178463128HCID 178463128, 화합물

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온도
110 °C

실험 절차

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.

후처리

  • 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
  • 출처 및 근거

    ORD 기록
    ord-eeac39b043c94603b833bbf96f10c563
    출처 데이터셋
    uspto-grants-1998_10
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05824802

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