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Hydrochloric Acid → 1-ethyl-4-fluoro-1H-pyrazole-5-carboxylic acid

HRID 244661
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 244661
[CH2:1]([N:3]1[C:7]([C:8]([O:10]CC)=[O:9])=[C:6]([F:13])[CH:5]=[N:4]1)[CH3:2].Cl>O1CCOCC1>[CH2:1]([N:3]1[C:7]([C:8]([OH:10])=[O:9])=[C:6]([F:13])[CH:5]=[N:4]1)[CH3:2]
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

4

Edukt 2

HCID 313Hydrochloric AcidHCID 58356399ethyl 1-ethyl-4-fluoro-1H-pyrazole-5-carboxylate

Produkt 1

HCID 583564401-ethyl-4-fluoro-1H-pyrazole-5-carboxylic acidAusbeute 45,7 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

To a solution of ethyl 1-ethyl-4-fluoro-1H-pyrazole-5-carboxylate (67 mg) in 1,4-dioxane (3 ml) was added 2M hydrochloric acid (2 ml) was added and the mixture was heated at reflux under nitrogen for 120 h. The mixture was cooled to room temperature and the solvent was removed in vacuo. Toluene (15 ml) was added and the solvent was removed in vacuo to give a solid that was dried in a vacuum oven overnight to give the title compound (26 mg) as a brown solid.

Aufarbeitung

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureat reflux under nitrogen for 120 h
  4. customthe solvent was removed in vacuo
  5. additionToluene (15 ml) was added
  6. customthe solvent was removed in vacuo
  7. customto give a solid
  8. customthat was dried in a vacuum oven overnight

Quellen und Nachweise

ORD-Eintrag
ord-11e4c56967834f96826b35e474adafa2
Quelldatensatz
uspto-grants-2014_02
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08658635B2

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