反应详情

0.60 g (1.1 mmol) of 1-methyl-2-[N-(4-amidinophenyl)aminomethyl]benzimidazol-5-yl-carboxylic acid-N-(2-pyridyl)-N-(2-ethoxycarbonylethyl)amide hydrochloride were added to about 30 mL of n-hexanol saturated with hydrogen chloride and the mixture was stirred for 19 hours at room temperature. Then the hexanol was distilled off in vacuo, the residue was mixed with about 5 mL of 1N ammonia solution with stirring, and evaporated down once more. The crude product thus obtained was purified by column chromatography (silica gel, dichloromethane/methanol=5:1). Yield: 53% of theory, C31H37N7O3 (555.7); Rf value: 0.36 (silica gel; dichloromethane/methanol=5:1); EKA mass spectrum: (M+H)+=556.

1. distillationThen the hexanol was distilled off in vacuo
2. additionthe residue was mixed with about 5 mL of 1N ammonia solution
3. stirringwith stirring
4. customevaporated down once more