反应详情

温度

0 °C

The compound (130 mg) obtained in Example 3-6 was dissolved in methanol (3.0 ml) and added with trimethyl orthoformate (0.130 ml) and 2-imidazole carboxaldehyde (37.3 mg) and the whole was stirred for 1 hour. After having been cooled to 0° C., the solution was added with sodium borohydride (21.5 mg) and stirred at room temperature for 3 hours. After completion of the reaction, the solvent was distilled off under reduced pressure and the residue was then dissolved in chloroform. The solution was washed with a 1 mol/l sodium hydroxide aqueous solution and then subjected to extraction with chloroform. The organic layer was washed with a saturated saline solution and then dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure. Then, the residue was purified through silica gel column chromatography (chloroform/methanol) and treated with hydrochloric acid, thereby obtaining a hydrochloride (16.4 mg) of the subject compound as a white solid.

1. stirringstirred at room temperature for 3 hours
2. customAfter completion of the reaction
3. distillationthe solvent was distilled off under reduced pressure
4. dissolutionthe residue was then dissolved in chloroform
5. washThe solution was washed with a 1 mol/l sodium hydroxide aqueous solution
6. extractionsubjected to extraction with chloroform
7. washThe organic layer was washed with a saturated saline solution
8. dry with materialdried with anhydrous sodium sulfate
9. filtrationAfter filtration
10. distillationthe solvent was distilled off under reduced pressure
11. customThen, the residue was purified through silica gel column chromatography (chloroform/methanol)
12. additiontreated with hydrochloric acid