反应详情

4.8 ml of aqueous potassium hydroxide solution (6M) were added to a solution of 600 mg (purity 93%, 2.22 mmol) of 4-iodo-6-methoxypyridin-3-ol in 4.8 ml of acetonitrile, the mixture was cooled in an ice bath and 863 μl (purity 75%, 3.56 mmol, 1.6 eq.) of difluoromethyl trifluoromethanesulphonate [Angew. Chem. Int. Ed. 2013, 52, 1-5; Journal of Fluorine Chemistry 2009, 130, 667-670] were added with vigorous stirring. The reaction mixture was stirred for 2 min and diluted with 33 ml of water. The aqueous phase was extracted twice with in each case 40 ml of diethyl ether. The combined organic phases were dried (sodium sulphate), filtered, concentrated under reduced pressure and dried. The crude product was purified by flash chromatography (IR-50SI, petroleum ether/ethyl acetate 12-20%). Yield: 407 mg (purity 90%, 55% of theory)

1. temperaturethe mixture was cooled in an ice bath
2. extractionThe aqueous phase was extracted twice with in each case 40 ml of diethyl ether
3. dry with materialThe combined organic phases were dried (sodium sulphate)
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. customdried
7. customThe crude product was purified by flash chromatography (IR-50SI, petroleum ether/ethyl acetate 12-20%)