反应详情

The compound (48.8 mg) obtained in Example 32-2 was dissolved in anhydrous methanol (1.0 ml) and then added with sodium cyanoborohydride (16.2 mg), trimethyl orthoformate (21.1 μl), propionaldehyde (13.9 μl), followed by stirring overnight at room temperature under a nitrogen atmosphere. After completion of the reaction, the solvent was distilled off and the residue was then dissolved in chloroform. A saturated aqueous sodium bicarbonate solution was added to the solution, followed by stirring. The resultant solution was subjected to extraction with chloroform and washed with a saturated aqueous sodium bicarbonate solution and saturated saline solution, and then the organic layer was dried with anhydrous sodium sulfate. The solvent was distilled off and the residue was then treated with hydrochloric acid. Subsequently, the treated product was purified through silica gel column chromatography (chloroform/methanol/water), thereby obtaining hydrochloride (33.2 mg) of the subject compound as a white solid.

1. customAfter completion of the reaction
2. distillationthe solvent was distilled off
3. dissolutionthe residue was then dissolved in chloroform
4. additionA saturated aqueous sodium bicarbonate solution was added to the solution
5. stirringby stirring
6. extractionThe resultant solution was subjected to extraction with chloroform
7. washwashed with a saturated aqueous sodium bicarbonate solution and saturated saline solution
8. dry with materialthe organic layer was dried with anhydrous sodium sulfate
9. distillationThe solvent was distilled off
10. additionthe residue was then treated with hydrochloric acid
11. customSubsequently, the treated product was purified through silica gel column chromatography (chloroform/methanol/water)