反应详情

To a solution of salicylic acid (1.38 g, 10 mmole) in tetrahydrofuran (40 mL) was added thionyl chloride (2.5 mL, 35 mmole) and refluxed 3 hr. The mixture was steamed (110° C.) by Dean-Stark. The residue was directly reacted with 4-chloro-2-fluorobenzenamine (1.1 mL, 10 mmole) in THF (40 mL) for 14 hr. The reaction mixture was concentrated and extracted with ethyl acetate, dried over anhydrous magnesium sulfate. Recrystallization of desired products from hot dichloromethane afforded the compound.

1. temperaturerefluxed 3 hr
2. custom(110° C.)
3. concentrationThe reaction mixture was concentrated
4. extractionextracted with ethyl acetate
5. dry with materialdried over anhydrous magnesium sulfate
6. customRecrystallization of desired products from hot dichloromethane
7. customafforded the compound