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Hydrochloric Acid → HCID 178418429, Verbindung

HRID 1813
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1813
[C:1]([C:3]1[C:7]([S:8][C:9]([F:12])([F:11])[F:10])=[C:6]([NH:13]C(=O)C(F)(F)F)[NH:5][N:4]=1)#[N:2].[OH-].[NH4+].Cl>CO.C(OCC)(=O)C>[C:1]([C:3]1[C:7]([S:8][C:9]([F:12])([F:11])[F:10])=[C:6]([NH2:13])[NH:5][N:4]=1)#[N:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

6

Edukt 3

HCID 313Hydrochloric AcidHCID 14923Ammonium HydroxideHCID 1784183603-cyano-4-trifluoromethylsulfenyl-5-(N-trifluoroacetylamino)pyrazole

Produkt 1

HCID 178418429HCID 178418429, VerbindungAusbeute 87,6 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 887MethanolLösungsmittel
HCID 8857
Ethyl Acetate
Lösungsmittel

Versuchsvorschrift

The product of Step E (55 g, 181 mmoles) was dissolved in methanol. 100 ml of ammonium hydroxide were added, the solution was refluxed for 3 hours and then stirred at room temperature for 15 hours. The methanolic solution was brought to pH7 using concentrated aqueous hydrochloric acid and diluted with ethyl acetate. The organic layer was washed several times with water and brine, dried over MgSO4 and concentrated to dryness to give an oily brown residue which was recrystallized from methyl tert-butyl ether to afford 33 g of the title compound, m.p. around 187° C.

Aufarbeitung

  1. temperaturethe solution was refluxed for 3 hours
  2. washThe organic layer was washed several times with water and brine
  3. dry with materialdried over MgSO4
  4. concentrationconcentrated to dryness
  5. customto give an oily brown residue which
  6. customwas recrystallized from methyl tert-butyl ether

Quellen und Nachweise

ORD-Eintrag
ord-519d1ed0c254438c8f86070fac54bfc1
Quelldatensatz
uspto-grants-1998_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US05726324

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