Water → HCID 22640034, compound

Participants

Reaction Steps

0.14 g (1.0 mmol) of dimedone and catalytic amount of tetrakis(triphenylphosphine)palladium(0) (12 mg) are added to a solution of 0.48 g (1.0 mmol) of [3-allyloxy-4-(3-nitro-imidazo[1,2-b]pyridazin-6-yloxy)-benzyl]-(5-chloro-2,6-dimethyl-pyrimidin-4-yl)-amine (from example A15) in 15 ml of dry toluene. The reaction mixture is refluxed under nitrogen for 1 h and then cooled to room temperature. The solution is poured into water (100 ml), extracted with ethyl acetate (4×100 ml) and the combined organic layers are dried with magnesium sulphate and concentrated in vacuo. The residue is crystallized from petroleum ether to give 0.44 g (50%) of the title compound as a beige powder of m.p. >114° C.

Provenance & Evidence