反应详情

温度

80 °C

A mixture of 1,2-dihydro-6-(4-fluorophenyl)-5-[4-(methylsulfonyl)phenyl]-2-oxo-pyridine-3-carbonitrile (Example 2, Step 3) (0.66 g, 1.81 mMol), 12 ml of 1,2,4-trimethylbenzene, 1.0 g of KBr, and 5 g of PBr5 was heated to 80° C. for 2 hours and then to 180° C. overnight. The reaction mixture was cooled to room temperature and stirred with 75 ml of water for 1 hour. The organic portion was extracted into dichloromethane. The dichloromethane extract was washed once with brine, dried over MgSO4, and evaporated to dryness. The residual oil was purified by HPLC to give 0.55 g (72% yield) of solid: m.p. 229.5°-231.5° C.

1. customto 180° C.
2. customovernight
3. temperatureThe reaction mixture was cooled to room temperature
4. extractionThe organic portion was extracted into dichloromethane
5. extractionThe dichloromethane extract
6. washwas washed once with brine
7. dry with materialdried over MgSO4
8. customevaporated to dryness
9. customThe residual oil was purified by HPLC