Reaktion #1533228

Reaktionsgleichung

cesium carbonate

2-bromo-3-(but-2-ynyl)-3,5-dihydro-imidazo[4,5-d]pyridazin-4-one

2-chloromethyl-4-methyl-quinazoline

→

2-bromo-3-(but-2-ynyl)-5-(4-methyl-quinazolin-2-ylmethyl)-3,5-dihydro-imidazo[4,5-d]pyridazin-4-one

Lösungsmittel

dimethylformamide

water

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturthe solution was cooled to approx. 10° C.
2. 2
   Sonstigethe precipitate formed
3. 3
   Filtrationfiltered
4. 4
   Sonstigedried
5. 5
   Sonstigepurified by column chromatography (silica gel; eluant: dichloromethane/ethanol 1:0->19:1)

Vorschrift

489 mg (1.5 mol) cesium carbonate were added to a solution of 300 mg (1.12 mmol) 2-bromo-3-(but-2-ynyl)-3,5-dihydro-imidazo[4,5-d]pyridazin-4-one and 344 mg (1.35 mmol) 2-chloromethyl-4-methyl-quinazoline in 4 ml of dimethylformamide and this mixture was stirred for 1 h under an argon atmosphere at 80° C. Then the mixture was diluted with 10 ml of water, the solution was cooled to approx. 10° C., the precipitate formed was suction filtered and dried and purified by column chromatography (silica gel; eluant: dichloromethane/ethanol 1:0->19:1).

Quelle