Hydrochloric Acid → 1,4-dimethyl-1H-pyrazole-5-carboxylic acid

HRID 244616Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 244616
[CH3:1][N:2]1[C:6]([C:7]([O:9]C)=[O:8])=[C:5]([CH3:11])[CH:4]=[N:3]1.Cl>O1CCOCC1.Cl>[CH3:1][N:2]1[C:6]([C:7]([OH:9])=[O:8])=[C:5]([CH3:11])[CH:4]=[N:3]1

Komponenten

5

Edukt 2

HCID 313Hydrochloric AcidHCID 20718564Methyl 1,4-dimethyl-1H-pyrazole-5-carboxylate

Produkt 1

HCID 6431501,4-dimethyl-1H-pyrazole-5-carboxylic acidAusbeute 84,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 313Hydrochloric AcidKatalysatorHCID 312751,4-DioxaneLösungsmittel

Versuchsvorschrift

Methyl 1,4-dimethyl-1H-pyrazole-5-carboxylate (171 mg) was dissolved in 1,4-dioxane (2 ml). Hydrochloric acid (2 ml) was added and the mixture was heated at reflux for 70 h. One drop of concentrated hydrochloric acid was added and the mixture heated at reflux for 45 h. The solution was left to cool and then the solvent was removed in vacuo. To the residue toluene (15 ml) was added and the solvent was removed in vacuo. The solid was dried in a vacuum oven overnight to give the title compound (132 mg) as a white solid.

Aufarbeitung

  1. temperaturethe mixture was heated
  2. temperatureat reflux for 70 h
  3. temperaturethe mixture heated
  4. temperatureat reflux for 45 h
  5. waitThe solution was left
  6. temperatureto cool
  7. customthe solvent was removed in vacuo
  8. additionTo the residue toluene (15 ml) was added
  9. customthe solvent was removed in vacuo
  10. customThe solid was dried in a vacuum oven overnight

Quellen und Nachweise

ORD-Eintrag
ord-c0a6b1aec4624c2a862162fb7c6c4ffa
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08658635B2

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