反应详情

To a stirred DMF (90 ml) in an ice bath, 4-(bromomethyl)-3,5-dichloro-2,6-difluoropyridine (20 g, 72 mmol) and sodium benzoate (15 g, 104 mmol) were added. After 1 hr., the mixture was stirred in a water bath for ca. 20 hr. The product was then extracted with ether, washed with water twice, dried with anhydrous magnesium sulfate, filtered, and evaporated in vacuo to give a light brown oil. The light brown oil was purified by silica gel column chromatography (eluent, ether:hexane (1:15) to afford 18.6 g (81%) of (3,5-dichloro-2,6-difluoropyridin-4-yl)methyl benzoate as a colorless oil. 1H NMR (200 MHz, CDCl3) δ 5.61 (2H, s), 7.40-7.64 (3H, m), 8.00-8.05 (2H, m).

1. extractionThe product was then extracted with ether
2. washwashed with water twice
3. dry with materialdried with anhydrous magnesium sulfate
4. filtrationfiltered
5. customevaporated in vacuo
6. customto give a light brown oil
7. customThe light brown oil was purified by silica gel column chromatography (eluent, ether:hexane (1:15)