反应详情

温度

100 °C

Ethyl 5-iodo-6-methyl-2-oxo-1-[3-(trifluoromethyl)phenyl]-1,2-dihydropyridine-3-carboxylate (2.6 g, 5.76 mmol), phenyltributylstannane (2.24 mg, 6.10 mmol), tetrakis(triphenylphosphine)palladium(0) (17.3 mg, 0.02 mmol), toluene (15 ml) and anhydrous DME (1.5 ml) were placed in a Schlenk vessel equipped with a magnetic stirring bar. The vessel was purged with argon, sealed and heated at 100° C. overnight. After cooling to room temperature, the mixture was partitioned between ethyl acetate and water. The organic layer was washed with water and brine, dried over sodium sulfate, filtered and concentrated in vacuo. The residue was purified by preparative HPLC to give the tide compound as a white solid (0.8 g, 35%). 1H NMR (CDCl3): δ 8.26 (1H, s); 7.72 (2H, m); 7.56 (1H, s); 7.51-7.36 (4H, m); 7.34-7.28 (2H, m); 4.37 (2H, q, J 7.1 Hz); 1.97 (3H, s); 1.37 (3H, t). APCI-MS m/z: 402.3 [MH+].

1. customequipped with a magnetic stirring bar
2. customThe vessel was purged with argon
3. customsealed
4. temperatureAfter cooling to room temperature
5. customthe mixture was partitioned between ethyl acetate and water
6. washThe organic layer was washed with water and brine
7. dry with materialdried over sodium sulfate
8. filtrationfiltered
9. concentrationconcentrated in vacuo
10. customThe residue was purified by preparative HPLC