Water → Methyl 5-(difluoromethoxy)-1-methyl-1H-pyrazole-3-carboxylate

HRID 362651Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 362651
[OH:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([O:10][CH3:11])=[O:9])[CH:3]=1.C(=O)([O-])[O-].[K+].[K+].Cl[CH:19]([F:21])[F:20].O>CN(C)C=O>[F:20][CH:19]([F:21])[O:1][C:2]1[N:6]([CH3:7])[N:5]=[C:4]([C:8]([O:10][CH3:11])=[O:9])[CH:3]=1

Komponenten

6

Edukt 4

HCID 962WaterHCID 6372ChlorodifluoromethaneHCID 11430Potassium CarbonateHCID 178498595HCID 178498595, Verbindung

Produkt 1

HCID 54319416Methyl 5-(difluoromethoxy)-1-methyl-1H-pyrazole-3-carboxylate

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6228DimethylformamideLösungsmittel

Reaktionsbedingungen

Temperatur
70 °C

Versuchsvorschrift

67.6 g (0.43 mol) 5-Hydroxy-3-methoxycarbonyl-1-methylpyrazole and 299.2 g (2.17 mol) potassium carbonate was dissolved in 1500 ml dimethylformamide and heated to 70° C. At this temperature chlorodifluoromethane was introduced over 2 hours and the mixture stirred at 80° C. for 1.5 hours. The reaction mixture was added to water and extracted 6 times with ethyl acetate. The combined organic phases were washed with saturated aqueous sodium chloride and dried over magnesium sulfate. The reaction solution was concentrated.

Aufarbeitung

  1. extractionextracted 6 times with ethyl acetate
  2. washThe combined organic phases were washed with saturated aqueous sodium chloride
  3. dry with materialdried over magnesium sulfate
  4. concentrationThe reaction solution was concentrated

Quellen und Nachweise

ORD-Eintrag
ord-00d102e2297d4b64bd63ab720ce4305c
Quelldatensatz
uspto-grants-1999_02
Patentnummer
US05869686

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