反应详情

The compound (191 mg) obtained in Example 15-5 was dissolved in anhydrous methanol (4.0 ml) and added with sodium cyanoborohydride (41.5 mg), acetic acid (0.50 ml), and the compound (71.4 mg) obtained in Example 16-1 and the whole was stirred at room temperature for 2 days under a nitrogen atmosphere. After completion of the reaction, the solvent was distilled off. The resultant was dissolved in chloroform and added with a 1 mol/l sodium hydroxide aqueous solution, followed by stirring for a while. Then, the solution was subjected to extraction with chloroform and washed with a saturated aqueous sodium hydrogen carbonate solution and a saturated saline solution. The organic layer was dried with anhydrous sodium sulfate and the solvent was distilled off. The residue was purified through silica gel column chromatography (chloroform/ethyl acetate) and treated with hydrochloric acid, thereby obtaining a hydrochloride (222 mg) of the subject compound as a white solid.

1. customAfter completion of the reaction
2. distillationthe solvent was distilled off
3. dissolutionThe resultant was dissolved in chloroform
4. additionadded with a 1 mol/l sodium hydroxide aqueous solution
5. extractionThen, the solution was subjected to extraction with chloroform
6. washwashed with a saturated aqueous sodium hydrogen carbonate solution
7. dry with materialThe organic layer was dried with anhydrous sodium sulfate
8. distillationthe solvent was distilled off
9. customThe residue was purified through silica gel column chromatography (chloroform/ethyl acetate)
10. additiontreated with hydrochloric acid