反应详情

The compound (380 mg) obtained in Example 18-3 was dissolved in DMF (7.6 ml) and 60% sodium hydride (60.0 mg) was added thereto, and the whole was stirred for 1 hour. After that, methyl iodide (213 mg) was gradually added thereto and the whole was stirred at room temperature for 2 hours. After completion of the reaction, the solvent was distilled off under reduced pressure. The residue was dissolved in chloroform and washed with a saturated aqueous sodium hydrogen carbonate 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 under reduced pressure. The residue was purified through silica gel column chromatography (chloroform/methanol/water), thereby obtaining the subject compound (83.0 mg) as a brown solid.

1. stirringthe whole was stirred at room temperature for 2 hours
2. customAfter completion of the reaction
3. distillationthe solvent was distilled off under reduced pressure
4. dissolutionThe residue was dissolved in chloroform
5. washwashed with a saturated aqueous sodium hydrogen carbonate 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 under reduced pressure
11. customThe residue was purified through silica gel column chromatography (chloroform/methanol/water)