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Chlorosulfonic acid → HCID 15220190, 화합물

HRID 583045
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HRID 583045 반응식
[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[CH:14][CH:13]=2)=[N:4][N:5]([CH3:11])[C:6]=1[O:7][CH:8]([F:10])[F:9].[Cl:19][S:20](O)(=[O:22])=[O:21]>>[Cl:1][C:2]1[C:3]([C:12]2[CH:17]=[CH:16][C:15]([Cl:18])=[C:14]([S:20]([Cl:19])(=[O:22])=[O:21])[CH:13]=2)=[N:4][N:5]([CH3:11])[C:6]=1[O:7][CH:8]([F:9])[F:10]
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참가 물질

3

반응물 2

HCID 24638Chlorosulfonic acidHCID 15220185HCID 15220185, 화합물

생성물 1

HCID 15220190HCID 15220190, 화합물

반응 조건

온도
130 °C

실험 절차

47.9 g (0.16 mol) of 4-chloro-3-(4-chlorophenyl)-5-difluoromethoxy-1-methyl-1H-pyrazole were added a little at a time at 0° C. to 91 ml of chlorosulfonic acid. The mixture was stirred at 130° C. for 4 hours and then cooled, and the solution was poured carefully into ice-water. Product dissolved in the aqueous phase was extracted twice with dichloromethane. The combined organic phases were subsequently washed with saturated sodium hydrogen carbonate solution and with sodium chloride solution, then dried over magnesium sulfate and finally concentrated. Yield: 47.9 g.

후처리

  1. temperaturecooled
  2. dissolution
Product dissolved in the aqueous phase
  • extractionwas extracted twice with dichloromethane
  • washThe combined organic phases were subsequently washed with saturated sodium hydrogen carbonate solution and with sodium chloride solution
  • dry with materialdried over magnesium sulfate
  • concentrationfinally concentrated
  • 출처 및 근거

    ORD 기록
    ord-3150176bc5f74a0fabfe4203ca242cb8
    출처 데이터셋
    uspto-grants-1999_07
    DOI
    10.6084/m9.figshare.5104873.v1
    특허 번호
    US05928999

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