Acetyl chloride → 5-Acetylamino-1-methyl-6-pyridazone

HRID 893182Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 893182
[C:1](Cl)(=[O:3])[CH3:2].[NH2:5][C:6]1[C:11](=[O:12])[N:10]([CH3:13])[N:9]=[CH:8][CH:7]=1>O1CCOCC1.N1C=CC=CC=1>[C:1]([NH:5][C:6]1[C:11](=[O:12])[N:10]([CH3:13])[N:9]=[CH:8][CH:7]=1)(=[O:3])[CH3:2]

Komponenten

5

Edukt 2

HCID 6367Acetyl chlorideHCID 131036364-Amino-2-methyl-2,3-dihydropyridazin-3-one

Produkt 1

HCID 146266165-Acetylamino-1-methyl-6-pyridazoneAusbeute 58 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 1049PyridineLösungsmittelHCID 312751,4-DioxaneLösungsmittel

Reaktionsbedingungen

Temperatur
25 °C

Versuchsvorschrift

A solution of 2.7 ml of acetyl chloride in 20 ml of dioxane was added dropwise to a solution of 4.0 g (0.032 mol) of 5-amino-1-methyl-6-pyridazone in 100 ml of pyridine. After stirring for 12 hours at 25° C., the solvent was distilled off under reduced pressure, and the residue was taken up with methylene chloride, washed with sodium bicarbonate solution and dried. After the solvent had been stripped off under reduced pressure and the residue stirred with a small amount of diisopropyl ether, there was obtained 3.1 g (58.0%) of 5-acetylamino-1-methyl-6-pyridazone (active ingredient 1.001) of melting point 152°-153° C.

Aufarbeitung

  1. distillationthe solvent was distilled off under reduced pressure
  2. washwashed with sodium bicarbonate solution
  3. customdried
  4. stirringthe residue stirred with a small amount of diisopropyl ether

Quellen und Nachweise

ORD-Eintrag
ord-30ab794546f0402a8858c5bd6768c80b
Quelldatensatz
uspto-grants-1992_06
Patentnummer
US05123952

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