Chloroform → HCID 19063122, compound

Participants

Reaction Steps

2.9 g of 4-amino-6,7-dimethoxy-2-(1-piperazinyl)-quinazoline (prepared according to: J. Med. Chem. 20, 146-149 (1977)) are added in little portions, in about 10' and at room temperature, to a solution of 4.2 g dicyclohexylcarbodiimide 97% and 0.12 g of 4-dimethylaminopyridine in 60 ml CHCl3. The mixture is stirred for 10' at the same temperature and added with 2.55 g of 2,2-diphenylacetic acid and again stirred for 6 h. The residue obtained after evaporation of the solvent is purified by flash chromatography on SiO2 column elating with CHCl3 /MeOH 100:2. The fractions containing the pure base are pooled, the solvents evaporated, the residue is dissolved in warm EtOH 95% and the solution treated with HCl in EtOH about 4N. The salt which crystallizes by cooling the solution is collected by filtration and recrystallized from EtOH 90% to give 3.2 g (60%) of the wanted compound; m.p.: 282°-283° C.

Provenance & Evidence