反应详情

The amine (prepared in reference example 3, 1.0 g) and 4-guanidinobenzoic acid hydrochloride (0.95 g) were dissolved in the mixture of pyridine (5 ml) and dimethylformamide (5 ml). Dicyclohexylcarbodiimide (0.91 g) was added to the solution. The mixture was stirred for 2.5 days. The reaction solution was fitered. The filtrate was evaporated. The residue was dissolved in methanol (10 ml), and 1N hydrochloric acid (6 ml) was added to the solution. The solution was evaporated. The residue was purified by column chromatography on silica gel (methylene chloride:methanol=10:1) to give the title compound (275 mg) having the following physical data.

1. customThe filtrate was evaporated
2. dissolutionThe residue was dissolved in methanol (10 ml)
3. addition1N hydrochloric acid (6 ml) was added to the solution
4. customThe solution was evaporated
5. customThe residue was purified by column chromatography on silica gel (methylene chloride:methanol=10:1)