Ethyl Acetoacetate → HCID 20361945, Verbindung

HRID 1415589Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1415589
C(O[C:4](=[O:9])[CH2:5][C:6]([CH3:8])=O)C.[CH3:10][CH:11]([NH:19][NH2:20])[C:12]1[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=1>C(O)C>[CH3:8][C:6]1[NH:20][N:19]([CH:11]([CH3:10])[C:12]2[CH:17]=[CH:16][C:15]([CH3:18])=[CH:14][CH:13]=2)[C:4](=[O:9])[CH:5]=1

Komponenten

4

Edukt 2

HCID 8868Ethyl AcetoacetateHCID 12489385HCID 12489385, Verbindung

Produkt 1

HCID 20361945HCID 20361945, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel2×

Versuchsvorschrift

26 g of acetoacetic acid ethyl ester were dissolved in 20 ml of absolute ethanol. 30.0 g of α-methyl-4-methylbenzylhydrazine in a little absolute ethanol were slowly added to this solution under nitrogen. After the exothermic reaction had subsided, the mixture was heated for 2 hours under reflux. On cooling, the crude product crystallized out and was purified by recrystallization from methanol. Melting point 144°- 146° C; yield 28 g (65% of theory).

Aufarbeitung

  1. customAfter the exothermic reaction
  2. temperaturethe mixture was heated for 2 hours
  3. temperatureunder reflux
  4. temperatureOn cooling
  5. customthe crude product crystallized out
  6. customwas purified by recrystallization from methanol

Quellen und Nachweise

ORD-Eintrag
ord-35cbb67878ec4f5f8aaea3b9826f4c29
Quelldatensatz
uspto-grants-1977_01
Patentnummer
US04005215

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