反应详情

温度

80 °C

To a solution of 4-bromo-3-fluorobenzoic acid (220 mg, 1.0 mmol) in dioxane/H2O (5:1, 12 mL) was added K2CO3 (414 mg, 3.0 mmol), tetrakistriphenylphosphine Pd(0) (58 mg, 0.05 mmol) and 5-(5,5-dimethyl-1,3,2-dioxaborinan-2-yl)-1-methyl-1H-pyrazole (214 mg, 1.1 mmol). The reaction mixture was heated to 80° C. in a sealed tube for 12 h and was then partitioned between 6N NaOH and DCM. The pH of the aqueous phase was adjusted to ˜3 with 3M HCl and washed several times with DCM. The combined organic fractions were dried (Na2SO4), concentrated under vacuum and used directly without further purification (196 mg, 89%): LC-MS (ES) m/z=221 (M+H)+.

1. customwas then partitioned between 6N NaOH and DCM
2. washwashed several times with DCM
3. dry with materialThe combined organic fractions were dried (Na2SO4)
4. concentrationconcentrated under vacuum
5. customused directly without further purification (196 mg, 89%)