Diethylamine → HCID 11009931, compound

Participants

Reaction Steps

10.4 ml of diethylamine in 10 ml of diethyl ether were added dropwise to a solution of 10.0 g of 2,4-dichloroquinazoline in 400 ml of diethyl ether and the mixture was stirred for 3 h at room temperature. After distillation of the solvent under vacuum, the residue was taken up with 200 ml of methanol and stirred with 10 g of basic ion exchanger (®Lewatit M600) for 3 h. The ion exchanger was filtered off and the filtrate was concentrated to dryness on a rotary evaporator. The residue was taken up with 200 ml of dichloromethane and the solution was washed with twice 50 ml of water. After the organic phase had been dried over magnesium sulfate and the solvent stripped off, the crude product was treated with 50 ml of diethyl ether/petroleum ether (1/1) and left to crystallize at 4° C. overnight.

Provenance & Evidence