Hydrochloric Acid → HCID 13798309, Verbindung

HRID 580258Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 580258
[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([O:9]S(C)(=O)=O)=[CH:4][C:3]=1[N:14]1[C:18]([CH3:19])=[C:17]([Cl:20])[C:16]([CH3:21])=[N:15]1.[OH-].[Na+].Cl>>[Cl:1][C:2]1[CH:7]=[C:6]([Cl:8])[C:5]([OH:9])=[CH:4][C:3]=1[N:14]1[C:18]([CH3:19])=[C:17]([Cl:20])[C:16]([CH3:21])=[N:15]1

Komponenten

4

Edukt 3

HCID 313Hydrochloric AcidHCID 14798Sodium HydroxideHCID 137983241-(2,4-Dichloro-5-methylsulfonyloxyphenyl)-3,5-dimethyl-4-chloropyrazole

Produkt 1

HCID 13798309HCID 13798309, VerbindungAusbeute 91,8 %

Reaktionsbedingungen

Temperatur
50 °C

Versuchsvorschrift

A mixture of 1-(2,4-dichloro-5-methylsulfonyloxyphenyl)-3,5-dimethyl-4-chloropyrazole (37.0 g) and 2N aqueous sodium hydroxide was stirred at 50° C. for 30 minutes. After cooling, the reaction mixture was acidified with aqueous hydrochloric acid and then extracted with toluene. The resulting toluene layer was washed with water and dried over anhydrous sodium sulfate. Removal of the solvent by distillation in vacuo gave the titled compound (26.8 g) as a pale yellow crystalline solid. Recrystallization of this solid from a mixture of n-hexane/ethyl acetate afforded a white crystalline solid. m.p. 172°-174° C.

Aufarbeitung

  1. temperatureAfter cooling
  2. extractionextracted with toluene
  3. washThe resulting toluene layer was washed with water
  4. dry with materialdried over anhydrous sodium sulfate
  5. customRemoval of the solvent
  6. distillationby distillation in vacuo

Quellen und Nachweise

ORD-Eintrag
ord-8d2a42dc8ee74778bdc0a69f6631eca3
Quelldatensatz
uspto-grants-1988_06
Patentnummer
US04752326

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