Water → HCID 14153048, compound

Participants

Reaction Steps

To a solution of 3.5 g. of the 5-(2-formylaminomethylprop-2-yl)-2-(6-hydroxypyridin-3-yl)-benzimidazole (prepared in Example 4d) in 20 ml. water and 13.6 ml. 1N potassium hydroxide solution in ethanol is added 0.85 ml. methyl iodide, while cooling with water. After 24 hours, it is filtered off with suction and purified by column chromatography (silica gel, elution agent dichloromethane:methanolic ammonia=20:1 v/v). Appropriate fractions are combined, the solvent is removed in a vacuum and the residue is digested with ethanol/water. After filtering off with suction, there are obtained 2.2 g. (57% of theory) of the title compound which, per mole, still contains 0.75 mole of water, as colourless crystals which, in the air, become reddish coloured; m.p. 217°-221° C.

Provenance & Evidence