Nitrogen → HCID 19379860, compound

Participants

Reaction Conditions

Reaction Steps

To 6-chloro-2-methoxycarbonyl-1-(4-fluorophenyl)-3-indolinon (7.5 g) in NMP (75 ml) was added MgCl2, 6H2O (9 g). The mixture was heated at 130° C. under N2 for one hour and finally the temperature was raised to 190° C. while H2O vapours were carried away by a gentle stream of N2. 1-[2-[3-(2-propyl)-2-imidazolidinon-1-yl]ethyl]-piperazine (12 g) in NMP (30 ml) were added and the temperature kept at 190°-200° C. for another hour. After cooling to room temperature the reaction mixture was poured into ethyl acetate (200 ml) and a saturated NH4Cl solution (500 ml) added. The organic phase was separated, dried (anh. MgSO4), filtered and the solvent evaporated. The remaining oil was purified by column chromatography on silica gel (eluent ethyl acetate/ethanol/triethylamine 90/10/4) yielding 5.7 g of pure title compound 6a. Mp: 176° -177° C.

Provenance & Evidence