反应详情

To a solution of dimethyl carbonate (30 mL, 0.36 mol) in dry THF (600 mL) was added sodium hydride (15 g, 0.36 mol) by portion at 5-10° C. The resulting mixture was stirred at this temperature for 30 min and then was added a solution of cyclooctanone (15.0 g, 0.12 mol) in THF (100 mL) dropwise over 30 min. The resultant mixture was stirred at refluxed for 4 h before cooling to room temperature. The reaction mixture was poured into saturated NaHCO3 solution (100 mL) and ice (500 g), and then the mixture was extracted with PE/EA (4:1, 400 mL×2). The organic layer was washed with brine (400 mL), dried over Na2SO4 and concentrated to give crude product. Then the target product (19.3 g, 88%) was purified by distilling at 60° C. in vacuum.

1. temperatureat refluxed for 4 h
2. extractionthe mixture was extracted with PE/EA (4:1, 400 mL×2)
3. washThe organic layer was washed with brine (400 mL)
4. dry with materialdried over Na2SO4
5. concentrationconcentrated
6. customto give crude product
7. customThen the target product (19.3 g, 88%) was purified
8. distillationby distilling at 60° C. in vacuum