反应详情

The compound (54.2 mg) obtained in Example 92-3 and the compound (76.8 mg) obtained in Example 84-5 were dissolved in ethanol (4.3 ml) and added with acetic acid (80 μl). The solution was added with sodium cyanoborohydride (49.6 mg) and the whole was stirred at room temperature for 1.5 hours. The solution was added with a 36% formaldehyde aqueous solution (0.10 ml) and the whole was stirred at room temperature for 1 hour. After completion of the reaction, the solvent was distilled off and the residue was dissolved in chloroform and washed with a 1 mol/l sodium hydroxide aqueous solution, followed by extraction with chloroform. The organic layer was washed with a saturated saline solution and dried with anhydrous sodium sulfate. After filtration, the solvent was distilled off and the residue was purified through silica gel column chromatography (chloroform), thereby obtaining the subject compound (94.9 mg) as a colorless oily substance.

1. stirringthe whole was stirred at room temperature for 1 hour
2. customAfter completion of the reaction
3. distillationthe solvent was distilled off
4. dissolutionthe residue was dissolved in chloroform
5. washwashed with a 1 mol/l sodium hydroxide aqueous solution
6. extractionfollowed by 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
11. customthe residue was purified through silica gel column chromatography (chloroform)