Methylamine → HCID 15222249, compound

Participants

Reaction Conditions

Reaction Steps

A suspension of 1.7 g (0.005 mol) of 7-chloro-9-methyl-2-phenyl-9H-imidazo[1,2-a]benzimidazole-3-acetic acid is prepared in 50 ml of dry tetrahydrofuran, 1.3 g (0.008 mol) of N,N'-carbonyldiimidazole are added thereto and the mixture is stirred at 40° C. for 2 h. The solution obtained is treated with an excess of dry gaseous methylamine and stirred for 72 h. The solvent is evaporated under reduced pressure. The residue is treated with 50 ml of water. The insoluble matter is separated by filtration, washed with water and then dried. 1.66 g of solid are obtained which are purified by silica gel chromatography, eluting with a dichloromethane/methanol 95/5 mixture. The product is recrystallized from an N,N-dimethylformamide/water 75/25 mixture and then dried. 1.27 g of solid are obtained. Melting point: 274°-275° C.

Provenance & Evidence