Reaktionsgleichung
[NH:1]([C:3]1[NH:12][C:11](=[O:13])[C:10]2[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=2)[N:4]=1)[NH2:2].CO[CH:16](OC)[CH2:17][C:18](=O)[CH3:19].Cl>C(O)C>[CH3:19][C:18]1[CH:17]=[CH:16][N:1]([C:3]2[NH:12][C:11](=[O:13])[C:10]3[C:5](=[CH:6][CH:7]=[CH:8][CH:9]=3)[N:4]=2)[N:2]=1Komponenten
5
Edukt 3
Produkt 1
Reagenzien, Katalysatoren, Lösungsmittel 1
Versuchsvorschrift
35.2 g (0.2 mole) of 2-hydrazino-4(3H)-quinazolinone, 500 ml of ethanol and 31.68 g (0.24 mole) of 4,4-dimethoxy-butan-2-one are boiled under reflux for 4.5 hours. The initial suspension has then dissolved. The same volume of 2 N HCl at 50° is added at 50°, whereupon a precipitate soon forms. After warming at 50° for a total of 40 minutes, the 2-(3-methyl-1H-pyrazol-1-yl)-4(3H)-quinazolinone is isolated by filtration with suction. The crude product (35.9 g of melting point 162° to 165° C.) is recrystallized from ethanol and then has a melting point of 165° to 166° C.
Aufarbeitung
- temperatureunder reflux for 4.5 hours
- temperatureAfter warming at 50° for a total of 40 minutes
Quellen und Nachweise
- ORD-Eintrag
- ord-2d330b0118dd4d29bb8bc8721630b65a
- Quelldatensatz
- uspto-grants-1987_02
- Patentnummer
- US04644000
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