Water → 3,4-Dichloro-1-methyl-5-(propylsulfanyl)-1H-pyrazole

HRID 1632729Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1632729
[CH2:1]([SH:4])[CH2:2][CH3:3].[OH-].[K+].[CH3:7][N:8]1[C:12](Cl)=[C:11]([Cl:14])[C:10]([Cl:15])=[N:9]1.O>CS(C)=O>[CH3:7][N:8]1[C:12]([S:4][CH2:1][CH2:2][CH3:3])=[C:11]([Cl:14])[C:10]([Cl:15])=[N:9]1

Komponenten

6

Edukt 4

HCID 962WaterHCID 7848Propyl mercaptanHCID 14797Potassium HydroxideHCID 14751841H-Pyrazole, 3,4,5-trichloro-1-methyl-

Produkt 1

HCID 133743743,4-Dichloro-1-methyl-5-(propylsulfanyl)-1H-pyrazole

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 679Dimethyl SulfoxideLösungsmittel

Reaktionsbedingungen

Temperatur
120 °C

Versuchsvorschrift

A stirred mixture of 4.9 g (0.064 moles) propanthiol and 3 g (0.054 moles) potassium hydroxide in 50 ml dimethylsulfoxide was heated (at about 120° C.) for thirty minutes. Then 10 g (0.054 moles) 1-methyl-3,4,5-trichloropyrazole was added in one portion. Heating (at about 120° C.) of the stirred reaction mixture was continued for about 6 hours. The reaction mixture was allowed to cool. The reaction mixture was added to water (about 50 ml); the resulting mixture was extracted with ether. The etheral phase was separated, washed with water twice, and dried over magnesium sulfate. The solvent was then stripped. The product was distilled out at 124° C. under high vacuum and heat.

Aufarbeitung

  1. temperatureHeating
  2. custom(at about 120° C.) of the stirred reaction mixture
  3. temperatureto cool
  4. extractionthe resulting mixture was extracted with ether
  5. customThe etheral phase was separated
  6. washwashed with water twice
  7. dry with materialdried over magnesium sulfate
  8. distillationThe product was distilled out at 124° C. under high vacuum
  9. temperatureheat

Quellen und Nachweise

ORD-Eintrag
ord-11451eb847714e94a1bc5d892792080c
Quelldatensatz
uspto-grants-1984_10
Patentnummer
US04477462

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