反应详情

The product (0.867 g) obtained in the above (2) is dissolved in dichloromethane (15 ml), and thereto are added methanol (1.5 ml), 4-dimethylaminopyridine (34 mg) and WSC.HCl (0.633 g) under ice-cooling. The mixture is stirred under ice-cooling for two hours, and then stirred at room temperature for 12 hours. The mixture is concentrated under reduced pressure to the volume of about 5 ml, and the residue is poured into water. The mixture is extracted three time with ethyl acetate, and the organic layer is washed 1N HCl (twice), a saturated aqueous sodium hydrogen carbonate solution (twice), and with a saturated brine (twice), and then dried over anhydrous magnesium sulfate. The desiccant is removed by filtration, and the filtrate is concentrated under reduced pressure to give the title compound (0.875 g).

1. temperaturecooling
2. temperaturecooling for two hours
3. stirringstirred at room temperature for 12 hours
4. concentrationThe mixture is concentrated under reduced pressure to the volume of about 5 ml
5. additionthe residue is poured into water
6. extractionThe mixture is extracted three time with ethyl acetate
7. washthe organic layer is washed 1N HCl (twice), a saturated aqueous sodium hydrogen carbonate solution (twice), and with a saturated brine (twice), and
8. dry with materialthen dried over anhydrous magnesium sulfate
9. customThe desiccant is removed by filtration
10. concentrationthe filtrate is concentrated under reduced pressure