Hydrochloric Acid → 5-(3-Methanesulfonyl-[1,2,4]triazol-4-yl)-2-methoxy-benzoic acid

HRID 2230746Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2230746
C[O:2][C:3](=[O:21])[C:4]1[CH:9]=[C:8]([N:10]2[CH:14]=[N:13][N:12]=[C:11]2[S:15]([CH3:18])(=[O:17])=[O:16])[CH:7]=[CH:6][C:5]=1[O:19][CH3:20].[OH-].[Li+].O.Cl>O1CCCC1>[CH3:18][S:15]([C:11]1[N:10]([C:8]2[CH:7]=[CH:6][C:5]([O:19][CH3:20])=[C:4]([CH:9]=2)[C:3]([OH:21])=[O:2])[CH:14]=[N:13][N:12]=1)(=[O:16])=[O:17]

Komponenten

6

Edukt 4

HCID 313Hydrochloric AcidHCID 962WaterHCID 3939Lithium HydroxideHCID 701493355-(3-Methanesulfonyl-[1,2,4]triazol-4-yl)-2-methoxy-benzoic acid methyl ester

Produkt 1

HCID 184644745-(3-Methanesulfonyl-[1,2,4]triazol-4-yl)-2-methoxy-benzoic acidAusbeute 83 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8028TetrahydrofuranLösungsmittel

Versuchsvorschrift

Stir a mixture of 5-(3-methanesulfonyl-[1,2,4]triazol-4-yl)-2-methoxy-benzoic acid methyl ester (1.0 g, 3.2 mmol), lithium hydroxide (0.042 g, 3.6 mmol), and 25% water in tetrahydrofuran (30 mL) at reflux overnight. Cool and add 1N hydrochloric acid (3.6 mL) dropwise via syringe. Concentrate to remove the tetrahydrofuran and collect the precipitate by vacuum filtration. Wash the filter cake twice with water and hexane, and dry in vacuo overnight to give 0.79 g of 5-(3-methanesulfonyl-[1,2,4]triazol-4-yl)-2-methoxy-benzoic acid as a solid.

Aufarbeitung

  1. temperatureat reflux overnight
  2. temperatureCool
  3. concentrationConcentrate
  4. customto remove the tetrahydrofuran
  5. customcollect the precipitate
  6. filtrationby vacuum filtration
  7. washWash the filter cake twice with water and hexane
  8. customdry in vacuo overnight

Quellen und Nachweise

ORD-Eintrag
ord-ffbfbe83fb4148829e060adf685ef166
Quelldatensatz
uspto-grants-2002_07
Patentnummer
US06423704B1

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