反应详情

温度

150 °C

2-Amino-5-iodo-pyridine (2.20 g; 10 mmol), sodium ethanethiolate 80% (1.7 g; 16 mmol) and copper powder (190 mg; 3.00 mmol) were loaded into a 100 mL round bottom flask under nitrogen. Ethylene glycol (40 mL; 0.25 mol) was added and the solution stirred at 150° C. for 26 h. The cooled solution was filtered and partitioned between ethyl acetate and water twice. The organic layer was dried over barium oxide, filtered and the solvent removed in vacuo to afford 1.2 g (yield 76%) of product as yellow oil. 1H-NMR (300 MHz; CDCl3), δ 8.06 (1H, d, 4JHH=2.1 Hz, Ar—H), 7.48 (1H, dd, 3JHH=8.7 Hz, 4JHH=2.4 Hz, Ar—H), 6.42 (1H, dd, 3JHH=8.7 Hz, 5JHH=0.6 Hz, Ar—H), 2.68 (2H, q, 3JHH=7.3 Hz, CH2), 1.15 (3H, t, 3JHH=7.2 Hz, CH3).

1. filtrationThe cooled solution was filtered
2. custompartitioned between ethyl acetate and water twice
3. dry with materialThe organic layer was dried over barium oxide
4. filtrationfiltered
5. customthe solvent removed in vacuo