反应详情

The compound (139.9 mg) obtained in Example 119-8 was dissolved in anhydrous THF (4.2 ml). Then, lithium aluminum hydride (68.3 mg) was added to the solution, followed by stirring at room temperature for 2 hours. The solution was added with an aqueous potassium sodium tartrate solution and stirred at room temperature. After completion of the reaction, extraction with chloroform was carried out. The organic layer was dried with magnesium sulfate and the solvent was then distilled off under reduced pressure. The residue was added with anhydrous methanol (4.1 ml), propionaldehyde (0.095 ml), trimethyl orthoformate (0.144 ml), and sodium cyanoborohydride (110.6 mg) and stirred at room temperature for 2 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. Then, the residue was dissolved in chloroform and washed with water, followed by drying with magnesium sulfate. The solvent was distilled off under reduced pressure. The residue was purified through silica gel column chromatography (toluene/ethyl acetate), thereby obtaining the subject compound (62.6 mg) as a yellow solid.

1. stirringstirred at room temperature
2. dry with materialThe organic layer was dried with magnesium sulfate
3. distillationthe solvent was then distilled off under reduced pressure
4. additionThe residue was added with anhydrous methanol (4.1 ml), propionaldehyde (0.095 ml), trimethyl orthoformate (0.144 ml), and sodium cyanoborohydride (110.6 mg)
5. stirringstirred at room temperature for 2 hours
6. customAfter completion of the reaction
7. distillationthe solvent was distilled off under reduced pressure
8. dissolutionThen, the residue was dissolved in chloroform
9. washwashed with water
10. dry with materialby drying with magnesium sulfate
11. distillationThe solvent was distilled off under reduced pressure
12. customThe residue was purified through silica gel column chromatography (toluene/ethyl acetate)