反应详情

温度

65 °C

A mixture of methyl 4′-amino-3-chlorobiphenyl-4-carboxylate (0.45 g, 1.7 mmol) and 2-chloro-6-fluoro-1,3-benzothiazole (0.32 g, 1.7 mmol) in n-butanol (8 mL) was heated to 60-70° C., and then 4N HCl in 1,4-dioxane (0.19 mL, 0.77 mmol) was added dropwise with stirring. The reaction mixture was heated at 90° C. for 18 h. Upon cooling to rt, the reaction mixture was concentrated under reduced pressure. The residue was triturated with ethanol, and the solid was collected by filtration. This yielded 0.399 g (56%) of the title compound as a beige solid. LC/MS m/z 411 (MH+), retention time 4.03 min. 1H NMR (400 MHz, DMSO-d6) δ 3.85 (s, 3H), 7.12 (t, 1H), 7.67-7.87 (m, 9H), 10.62 (br, 1H).

1. temperatureThe reaction mixture was heated at 90° C. for 18 h
2. temperatureUpon cooling to rt
3. concentrationthe reaction mixture was concentrated under reduced pressure
4. customThe residue was triturated with ethanol
5. filtrationthe solid was collected by filtration