HCID 6481592, compound → HCID 67053684, compound

Participants

Reaction Conditions

Reaction Steps

A mixture of 3-{4-[1-(3-Hydroxy-6-methyl-pyridin-2-ylmethyl)-4,6-dimethyl-1H-benzoimidazol-2-ylamino]-piperidin-1-yl}-propionic acid ethyl ester (0.0065 mol) in methanol/NH3 7N (15 ml) was stirred in a sealed vessel at 70° C. for 12 hours. The solvent was evaporated until dryness. The residue (0.3 g) was purified by column chromatography over silica gel (eluent: CH2Cl2/CH3OH/NH4OH 85/14/1; 5 μm). The pure fractions were collected and the solvent was evaporated. The residue (0.09 g, 32%) was crystallized from diisopropylether. The precipitate was filtered off and dried, yielding 0.086 g of 3-{4-[1-(3-hydroxy-6-methyl-pyridin-2-ylmethyl)-4,6-dimethyl-1H-benzoimidazol-2-ylamino]-piperidin-1-yl}-propionamide (compound 5, 30%, melting point: 212° C.).

Provenance & Evidence