反应详情

2,2-Dimethylcyclopentane-1,3-dicarboxylic anhydride (1.68 g., 10 mmole) and 1-(4-aminobutyl)-4-(2-pyrimidinyl)piperazine (2.55 g., 11 mmole) were combined in 500 ml. of xylene and refluxed for 48 hours with water removal via a Dean-Stark trap. The solvent was removed in vacuo and the residue column chromatographed on 100 g. of silica gel using a gradient elution from straight chloroform to 5% ethanol/chloroform. Concentration of the product in vacuum and recrystallization from isopropanol with addition of 4N isopropanolic HCl and acetone gave 600 mg. of the title compound as the dihydrochloride, monohydrate; m.p. 227°-229° C. (d).

1. customThe solvent was removed in vacuo
2. customthe residue column chromatographed on 100 g
3. washof silica gel using a gradient elution from straight chloroform to 5% ethanol/chloroform
4. customConcentration of the product in vacuum and recrystallization from isopropanol
5. additionwith addition of 4N isopropanolic HCl and acetone
6. customgave 600 mg