Methylhydrazine → HCID 13949475, Verbindung

HRID 1022400Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1022400
Cl[C:2]1[N:11]=[C:10]([C:12]2[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=2)[C:9]2[C:4](=[CH:5][CH:6]=[C:7]([Cl:18])[CH:8]=2)[N:3]=1.[CH3:19][NH:20][NH2:21]>O>[Cl:18][C:7]1[CH:8]=[C:9]2[C:4](=[CH:5][CH:6]=1)[N:3]=[C:2]([N:20]([CH3:19])[NH2:21])[N:11]=[C:10]2[C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][CH:13]=1

Komponenten

4

Edukt 2

HCID 6061MethylhydrazineHCID 16282212,6-dichloro-4-phenylquinazoline

Produkt 1

HCID 13949475HCID 13949475, VerbindungAusbeute 79,1 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Versuchsvorschrift

A mixture of 275 mg of 2,6-dichloro-4-phenylquinazoline (compound No. Ia1-3) and 461 mg of monomethylhydrazine was stirred at 85° C. for 30 minutes. The resulting reaction product was cooled and 200 ml of water was added thereto. Precipitated crystals were collected by filtration and the collected product was purified by column chromatography (ethyl acetate) to obtain 225 mg of the titled compound. Mp. 155.9° C. 1H NMR (CDCl3): 3.52 (3H, s), 4.65 (2H, s), 7.54-7.63 (5H, m), 7.70-7.74 (2H, m), 7.80 (1H, d, J=2.0 Hz).

Aufarbeitung

  1. customThe resulting reaction product
  2. temperaturewas cooled
  3. customPrecipitated crystals
  4. filtrationwere collected by filtration
  5. customthe collected product was purified by column chromatography (ethyl acetate)

Quellen und Nachweise

ORD-Eintrag
ord-ebfde4168a804d758631345bd0eec041
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08722580B2

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