Trifluoroacetic acid → 5-chloro-3-(trifluoromethyl)-1H-pyrazole

HRID 238673Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 238673
[Cl:1][C:2]1[N:6](S(N(C)C)(=O)=O)[N:5]=[C:4]([C:13]([F:16])([F:15])[F:14])[CH:3]=1.FC(F)(F)C(O)=O>O.C(=O)([O-])[O-].[Na+].[Na+]>[Cl:1][C:2]1[NH:6][N:5]=[C:4]([C:13]([F:16])([F:15])[F:14])[CH:3]=1

Komponenten

5

Edukt 2

HCID 6422Trifluoroacetic acidHCID 674628085-chloro-N,N-dimethyl-3-(trifluoromethyl)-1H-pyrazole-1-sulfonamide2×

Produkt 1

HCID 1785061975-chloro-3-(trifluoromethyl)-1H-pyrazole

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 962WaterLösungsmittelHCID 10340Sodium CarbonateLösungsmittel

Versuchsvorschrift

A solution of 5-chloro-N,N-dimethyl-3-(trifluoromethyl)-1H-pyrazole-1-sulfonamide (i.e. the product of Example 10, Step B) (4.38 g, 15.8 mmol) and trifluoroacetic acid (2.7 mL, 35 mmol) was stirred at 0° C. for 1.5 h. The reaction mixture was diluted with water (15 mL), and sodium carbonate was added to raise the pH to 12. The solution was extracted with diethyl ether, dried (MgSO4), and concentrated under reduced pressure to give 2.1 g of the title compound. This compound was of sufficient purity to use in subsequent reactions.

Aufarbeitung

  1. additionwas added
  2. temperatureto raise the pH to 12
  3. extractionThe solution was extracted with diethyl ether
  4. dry with materialdried (MgSO4)
  5. concentrationconcentrated under reduced pressure

Quellen und Nachweise

ORD-Eintrag
ord-cede304086f944cc80ebed391f7dfdf4
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08642634B2

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