反应详情

The compound (231 mg) obtained in Example 76-4 was dissolved in anhydrous methanol (5.0 ml) and added with sodium cyanoborohydride (61.6 mg), acetic acid (2.00 ml), and 1-methyl-2-imidazole carboxaldehyde (80.9 mg). The whole was stirred at room temperature for 6 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 saturated aqueous sodium hydrogen carbonate solution and the whole was stirred for a while. 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. The solvent was distilled off. The residue was purified through silica gel column chromatography (chloroform/methanol/water), thereby obtaining the subject compound (197 mg) as a colorless oily substance.

1. customAfter completion of the reaction
2. distillationthe solvent was distilled off
3. dissolutionThe resultant was dissolved in chloroform
4. additionadded with a saturated aqueous sodium hydrogen carbonate solution
5. stirringthe whole was stirred for a while
6. extractionThe solution was subjected to extraction with chloroform
7. washwashed with a saturated aqueous sodium hydrogen carbonate solution
8. dry with materialThe organic layer was dried with anhydrous sodium sulfate
9. distillationThe solvent was distilled off
10. customThe residue was purified through silica gel column chromatography (chloroform/methanol/water)