反应详情

To a solution of 2-amino-4-chloropyridine (150 g, 0.78 mol) in DMF (1.5 L) was added NIS (341 g, 1.52 mol) and the reaction mixture stirred at RT for 18 h before being concentrated in vacuo to 300 mL volume. The resultant residue was poured into 10% aqueous sodium thiosulfate solution (1.2 L), stirred for 15 min and the precipitate formed collected by filtration, washed with water then dried at 35° C. in vacuo to give the title compound as a pale brown solid (185 g, 62%). 1H NMR 400 MHz (CDCl3) δ: 8.33 (1H, s), 6.68 (1H, s), 4.52 (2H, s).

1. concentrationbefore being concentrated in vacuo to 300 mL volume
2. additionThe resultant residue was poured into 10% aqueous sodium thiosulfate solution (1.2 L)
3. stirringstirred for 15 min
4. customthe precipitate formed
5. filtrationcollected by filtration
6. washwashed with water
7. customthen dried at 35° C. in vacuo