反应详情

温度

0 °C

The compound (64.0 mg) obtained in Example 126-1 was dissolved in methanol (1.3 ml) and added with acetic acid (0.065 ml) and 1-methyl-2-imidazole carboxaldehyde (16.6 mg), followed by cooling to 0° C. Then, the solution was added with sodium cyanoborohydride (14.2 mg) and stirred at room temperature for 2 days. After completion of the reaction, the solvent was distilled off under reduced pressure and the residue was then dissolved in chloroform. After washing with a 1 mol/l sodium hydroxide aqueous solution, the solution was subjected to extraction with chloroform. The organic layer was washed with saturated saline solution and dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off under reduced pressure. Subsequently, the residue was purified through silica gel column chromatography (chloroform/methanol) and treated with hydrochloric acid, thereby obtaining hydrochloride (30.0 mg) of the subject compound as a white solid.

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