Hydrochloric Acid → 1,4-Dimethyl-1H-pyrazole-3-carboxylic acid

HRID 244687Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 244687
[OH-].[Li+].C1COCC1.[CH3:8][N:9]1[CH:13]=[C:12]([CH3:14])[C:11]([C:15]([O:17]C)=[O:16])=[N:10]1.Cl>O>[CH3:8][N:9]1[CH:13]=[C:12]([CH3:14])[C:11]([C:15]([OH:17])=[O:16])=[N:10]1

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 3939Lithium HydroxideHCID 8028TetrahydrofuranHCID 20718566methyl 1,4-dimethyl-1H-pyrazole-3-carboxylate

Produkt 1

HCID 53256851,4-Dimethyl-1H-pyrazole-3-carboxylic acid

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

Lithium hydroxide (0.864 g), THF (30 ml) and water (30 ml) were added to methyl 1,4-dimethyl-1H-pyrazole-3-carboxylate (1.39 g) and the reaction was stirred at room temperature for 3 h. The reaction was acidified with 5M HCl (aq) to pH to 7 and then washed through a waters HLB OASIS cation exchange cartridge. The cartridge was preconditioned with methanol, then water. The reaction was loaded onto the cartridge and washed with water, then eluted with methanol. The methanol fraction was evaporated in vacuo to give title compound, 1.1 g.

Aufarbeitung

  1. washwashed through a waters HLB OASIS cation exchange cartridge
  2. washwashed with water
  3. washeluted with methanol
  4. customThe methanol fraction was evaporated in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-96d268033c7b46709567f9bdc6904a32
Quelldatensatz
uspto-grants-2014_02
Patentnummer
US08658635B2

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