Hydrazine hydrate (1:1) → 6-(4-benzylamino-3-hydroxy-phenyl)-5-methyl-4,5-dihydro-2H-pyridazin-3-one

HRID 1619966Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1619966
O.[NH2:2][NH2:3].[CH2:4]([NH:11][C:12]1[CH:17]=[CH:16][C:15]([C:18](=O)[CH:19]([CH3:24])[CH2:20][C:21](O)=[O:22])=[CH:14][C:13]=1[OH:26])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1>C(O)(=O)C>[CH2:4]([NH:11][C:12]1[CH:17]=[CH:16][C:15]([C:18]2[CH:19]([CH3:24])[CH2:20][C:21](=[O:22])[NH:2][N:3]=2)=[CH:14][C:13]=1[OH:26])[C:5]1[CH:10]=[CH:9][CH:8]=[CH:7][CH:6]=1

Komponenten

4

Edukt 2

HCID 24654Hydrazine hydrate (1:1)HCID 674661774-(4-Benzylamino-3-hydroxy-phenyl)-3-methyl-4-oxo-butyric acid

Produkt 1

HCID 674671166-(4-benzylamino-3-hydroxy-phenyl)-5-methyl-4,5-dihydro-2H-pyridazin-3-one

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 176Acetic AcidLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

While cooling with the ice bath 69.9 ml (1396 mmol) hydrazine hydrate are added dropwise to 220 ml glacial acetic acid, then 54.7 g (175 mmol) 4-(4-benzylamino-3-hydroxy-phenyl)-3-methyl-4-oxo-butyric acid are added and the mixture is stirred for 1.5 h at 110° C. Then the mixture is cooled somewhat and poured onto ice water, the precipitated product is suction filtered, washed first with copious amounts of water, then with a little acetone and then dried in the vacuum dryer.

Aufarbeitung

  1. temperatureThen the mixture is cooled somewhat
  2. additionpoured onto ice water
  3. filtrationfiltered
  4. washwashed first with copious amounts of water
  5. dry with materialwith a little acetone and then dried in the vacuum dryer

Quellen und Nachweise

ORD-Eintrag
ord-01efdea66a83440794839b1af17bcc3a
Quelldatensatz
uspto-grants-2014_07
Patentnummer
US08772323B2

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