反应详情

The compound (0.40 g, 1.26 mmol) prepared in Step 1 of Example 9, methyl iodide (535.68 mg, 3.77 mmol), and DMF (10 mL) were charged to a dry round-bottom flask, and Cs2CO3 (0.82 g, 2.52 mmol) was added thereto with stirring. The reaction mixture was stirred at 50° C. for 3 hours. After the reaction was completed, the reaction liquid was transferred to an Erlenmeyer flask, and the reaction container was washed with methylene chloride. The reaction contents were combined and acidified with 2M-HCl on ice water. After being warmed to room temperature, CH2Cl2 (20 mL) and water (10 mL) were added and the reaction liquid was repeatedly extracted with methylene chloride. The organic layer was combined, washed with water and brine, and then dried over anhydrous Na2SO4. The solvent was removed under reduced pressure. Ethanol was added to the resulting sludge-like material, followed by trituration, and the resulting solid was filtered to give a white solid compound (0.41 g, 97.3%).

1. stirringThe reaction mixture was stirred at 50° C. for 3 hours
2. customthe reaction liquid
3. washthe reaction container was washed with methylene chloride
4. customThe reaction contents
5. customthe reaction liquid
6. extractionwas repeatedly extracted with methylene chloride
7. washwashed with water and brine
8. dry with materialdried over anhydrous Na2SO4
9. customThe solvent was removed under reduced pressure
10. additionEthanol was added to the resulting sludge-like material
11. filtrationthe resulting solid was filtered