反应详情

To 5-(2-chloro-4-methoxy-phenyl)-2-trifluoromethylisonicotinonitrile (0.7 g, 2.24 mmol) in chloroform (6 mL), was added to ClSO3H (0.62 mL). The solution was stirred at rt for 16 hrs. The solvent was removed and MeCN (3 mL) was added, followed by addition of POCl3 (3 mL). The mixture was heated at 60° C. for 16 hrs, then concentrated. The remainder was poured into ice water with stirring. The resulting solid was filtered, dried in vacuo over 2 days to yield 4-chloro-5-(4-cyano-6-trifluoromethyl-pyridin-3-yl)-2-methoxy-benzenesulfonyl chloride (0.79 g) as a pale yellow solid. tR=2.92 min (method 1).

1. customThe solvent was removed
2. additionMeCN (3 mL) was added
3. additionfollowed by addition of POCl3 (3 mL)
4. temperatureThe mixture was heated at 60° C. for 16 hrs
5. concentrationconcentrated
6. additionThe remainder was poured into ice water
7. stirringwith stirring
8. filtrationThe resulting solid was filtered
9. customdried in vacuo over 2 days