反应详情

The compound (31.2 mg) obtained in Example 18-6 was dissolved in methanol (1.0 ml) and added with acetic acid (30 μl) and 1-methyl-2-aminomethylimidazole (15.4 mg), and the whole was stirred at room temperature for 2 hours. Sodium cyanoborohydride (22.7 mg) was added thereto and the whole was stirred at room temperature for 15 hours. Furthermore, 2-imidazole carboxaldehyde (18.0 mg) was added thereto and the whole was stirred at room temperature for 18 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was dissolved in chloroform, washed with a saturated aqueous sodium hydrogen carbonate solution and a saturated saline solution, and dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure. The residue was purified through silica gel column chromatography (chloroform/methanol) and treated with hydrochloric acid, thereby obtaining a hydrochloride (25.6 mg) of the subject compound as a white solid.

1. stirringthe whole was stirred at room temperature for 15 hours
2. stirringthe whole was stirred at room temperature for 18 hours
3. customAfter completion of the reaction
4. distillationthe solvent was distilled off under reduced pressure
5. dissolutionThe residue was dissolved in chloroform
6. washwashed with a saturated aqueous sodium hydrogen carbonate solution
7. dry with materiala saturated saline solution, and dried with anhydrous sodium sulfate
8. filtrationAfter filtration
9. distillationthe solvent was distilled off under reduced pressure
10. customThe residue was purified through silica gel column chromatography (chloroform/methanol)
11. additiontreated with hydrochloric acid