Potassium Hydroxide → 2-(3,5-Dimethyl-1H-pyrazol-1-yl)benzene-1,3-diol

HRID 337344Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 337344
CC1C=CC(S([O:11][C:12]2[CH:17]=[CH:16][CH:15]=[C:14]([OH:18])[C:13]=2[N:19]2[C:23]([CH3:24])=[CH:22][C:21]([CH3:25])=[N:20]2)(=O)=O)=CC=1.[OH-].[K+]>C(O)C.O>[CH3:25][C:21]1[CH:22]=[C:23]([CH3:24])[N:19]([C:13]2[C:14]([OH:18])=[CH:15][CH:16]=[CH:17][C:12]=2[OH:11])[N:20]=1

Komponenten

5

Edukt 2

HCID 14797Potassium HydroxideHCID 867032542-(3,5-Dimethyl-1H-pyrazol-1-yl)-3-hydroxyphenyl 4-methylbenzenesulfonate

Produkt 1

HCID 601438812-(3,5-Dimethyl-1H-pyrazol-1-yl)benzene-1,3-diolAusbeute 58,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 962WaterLösungsmittel2×

Versuchsvorschrift

To 62 mg of 2-(3,5-dimethyl-1H-pyrazol-1-yl)-3-hydroxyphenyl 4-methylbenzene sulfonate was added a solution in which 97 mg of potassium hydroxide was dissolved in 1.5 ml of ethanol and 1.5 ml of water, and heated at reflux for 3.5 hours. To the reaction mixture, 20 ml of water was added, and extracted with 20 ml of ethyl acetate. After the organic layer was dried over anhydrous magnesium sulfate, the solvent was distilled off under reduced pressure, and purified using preparative thin-layer silica gel column chromatography (hexane:ethyl acetate=1:1) to yield 20.8 mg of the title compound.

Aufarbeitung

  1. temperatureat reflux for 3.5 hours
  2. extractionextracted with 20 ml of ethyl acetate
  3. dry with materialAfter the organic layer was dried over anhydrous magnesium sulfate
  4. distillationthe solvent was distilled off under reduced pressure
  5. custompurified

Quellen und Nachweise

ORD-Eintrag
ord-85206d9f8af0439a8851e6e3c895e74a
Quelldatensatz
uspto-grants-2014_11
Patentnummer
US08889727B2

Notizen zur Reaktion

Wird geladen…