反应详情

To 10.3 g (20.6 mmol) of ethyl 5-(3-cyclopropylmethoxy-4-difluoromethoxyphenyl)-2-(4-methoxybenzyloxymethyl)-1H-pyrrol-3-carboxylate obtained in Reference example 45-(c) were added 100 ml of dichloromethane and 10 ml of water, then, 5.15 g (22.7 mmol) of 2,3-dichloro-5,6-dicyano-1,4-benzoquinone was added to the mixture under ice-cooling, and the mixture was stirred at room temperature for 3 hours. After completion of the reaction, the reaction suspension was filtered through Celite, the filtrate was successively washed with a saturated aqueous solution of sodium hydrogencarbonate, and then, with a saturated aqueous solution of sodium chloride. The organic layer after separation was dried over anhydrous magnesium sulfate and then concentrated under reduced pressure. To the obtained concentrate was added 100 ml of a mixed solvent (diisopropyl ether/hexane=1/1 (V/V)), and the precipitated solid was collected by filtration. The obtained solid was washed with diisopropyl ether, and dried under reduced pressure to obtain 3.98 g of the title compound as a pale yellowish solid. (Yield: 49%)

1. temperaturecooling
2. customAfter completion of the reaction
3. filtrationthe reaction suspension was filtered through Celite
4. washthe filtrate was successively washed with a saturated aqueous solution of sodium hydrogencarbonate
5. customThe organic layer after separation
6. dry with materialwas dried over anhydrous magnesium sulfate
7. concentrationconcentrated under reduced pressure
8. concentrationTo the obtained concentrate
9. additionwas added 100 ml of a mixed solvent (diisopropyl ether/hexane=1/1 (V/V))
10. filtrationthe precipitated solid was collected by filtration
11. washThe obtained solid was washed with diisopropyl ether
12. customdried under reduced pressure