反应详情

To the solution of 4-(4-amino-3-methylphenoxy)-N-methylpicolinamide (25 mg, 0.097 mmol, 1.0 eq) in 1 mL of cold acetic acid was added ammonium thiocyanate (11 mg, 0.145 mmol, 1.5 eq). After stirring for a few minutes, bromine (6 μL, 0.116 mmol, 1.2 eq) was injected dropwise and reaction stirred at room temperature for 3 hours. Thereafter, reaction was quenched with NaHCO3 saturated solution (ca. 10 mL) and extracted with ethyl acetate (ca. 25 mL×3), combined organic extracts were dried over sodium sulfate and condensed under reduced pressure to give sufficiently pure crude product which was carried to next step without further purification. LC/MS (m/z) [315.1] (MH+).

1. customreaction
2. stirringstirred at room temperature for 3 hours
3. customThereafter, reaction
4. customwas quenched with NaHCO3 saturated solution (ca. 10 mL)
5. extractionextracted with ethyl acetate (ca. 25 mL×3)
6. dry with materialwere dried over sodium sulfate and condensed under reduced pressure
7. customto give sufficiently pure crude product which
8. customwas carried to next step without further purification