Reaktion #355449

Reaktionsgleichung

3-aminoacetophenone

compound

9-Anilino-7-methyl-1H-imidazo[4,5-f]quinoline Hydrochloride

→

9-(m-Acetylanilino)-7-methyl-1H-imidazo[4,5-f]quinoline Hydrochloride Hemihydrate

Lösungsmittel

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   workup.ADDITIONA mixture of 13.5 g
2. 2
   Temperaturat reflux overnight
3. 3
   EinengenThe solution was concentrated in vacuo
4. 4
   Sonstigeto give 30 g
5. 5
   SonstigeThe crude product was recrystallized from 1000 ml
6. 6
   SonstigeThe product was oven-dried (100°C)
7. 7
   Sonstigeto yield 24 g
8. 8
   Sonstigem.p. 225° -228°, completely 251°C.

Vorschrift

A mixture of 13.5 g. (0.1 m.) of 3-aminoacetophenone, 21.7 g. (0.1 m.) of the compound of Example I, C. and 500 ml. of ethanol was heated at reflux overnight with stirring. The solution was concentrated in vacuo to give 30 g. m.p. 156°-223°C. The crude product was recrystallized from 1000 ml. of MeOH, followed by concentration of the filtrate to the cloud point. The product was oven-dried (100°C) to yield 24 g. m.p. 225° -228°, completely 251°C.

Quelle