反应详情

温度

150 °C

To a 5 mL microwave vial was added methyl 4-amino-6-bromo-3-chloro-5-fluoropicolinate (200 mg, 1.0 mmol), benzo[d]thiazol-5-ylboronic acid (237 mg, 1.35 mmol), potassium fluoride (KF; 122 mg, 2.12 mmol), TPPTS-Na (tris-(3-sulfornatophenyl)-phosphine4-hydrate sodium salt, 67 mg, 0.106 mmol) and Pd(OAc)2 (11 mg, 0.053 mmol). Subsequently, CH3CN (1.0 mL) and H2O (3.0 mL) were added, and the reaction vial was sealed and heated in a Biotage microwave at 150° C. for 5 min, with external IR-sensor temperature monitoring from the side of the vessel. The reaction mixture was cooled to room temperature and diluted with dicloromethane, and washed wth water. The organic extracts were combined, dried (Na2SO4), filtered, and concentrated in vacuo. The crude product was purified by triturating with Et2O to yield the title compound as a brown solid (172 mg, 51%).

1. customthe reaction
2. customvial was sealed
3. temperatureThe reaction mixture was cooled to room temperature
4. washwashed wth water
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated in vacuo
8. customThe crude product was purified
9. customby triturating with Et2O