Ethanol → 4-Chloro-2-(4-chlorophenyl)-5-hydroxypyridazin-3(2H)-one

HRID 1165425

Reaktionsgleichung

Reaktionsgleichung von HRID 1165425
[OH-].[K+].[Cl:3][C:4]1[C:5](=[O:18])[N:6]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)[N:7]=[CH:8][C:9]=1Cl.C([OH:21])C>O>[Cl:3][C:4]1[C:5](=[O:18])[N:6]([C:11]2[CH:16]=[CH:15][C:14]([Cl:17])=[CH:13][CH:12]=2)[N:7]=[CH:8][C:9]=1[OH:21]

Komponenten

5

Edukt 3

HCID 702EthanolHCID 14797Potassium HydroxideHCID 7794024,5-Dichloro-2-(4-chlorophenyl)-3(2H)-pyridazinone

Produkt 1

HCID 546974414-Chloro-2-(4-chlorophenyl)-5-hydroxypyridazin-3(2H)-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

In 140 ml of water was dissolved 18.3 g (0.28 mol) of potassium hydroxide, and thereto were added 25.6 g (0.093 mol) of 4,5-dichloro-2-(4-chlorophenyl)-3(2H)-pyridazinone and 140 ml of ethanol. The reaction mixture was refluxed for 6 hours. After allowing to cool, ethanol was distilled off from the mixture under reduced pressure and then 300 of water was added to the mixture. Insoluble matter was removed by filtration and filtrate was acidified with hydrochloric acid. The solid thus precipitated was taken out by filtration, washed with water, and recrystallized from ethanol to give 11.1 g of the intended compound having melting point (hereinafter referred to as "m.p.") of 270°-271° C.

Aufarbeitung

  1. temperatureThe reaction mixture was refluxed for 6 hours
  2. temperatureto cool
  3. distillationethanol was distilled off from the mixture under reduced pressure
  4. addition300 of water was added to the mixture
  5. customInsoluble matter was removed by filtration and filtrate
  6. customThe solid thus precipitated
  7. filtrationwas taken out by filtration
  8. washwashed with water
  9. customrecrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-31fcf984d4d147f0a84abe9d0f46f7ec
Quelldatensatz
uspto-grants-1990_03
Patentnummer
US04910201

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