反应详情

温度

80 °C

To a solution of 4,5-dibromo-2-thiophenecarboxylic acid (3.30 g, 11.54 mmol) in dioxane/H2O (4:1, 100 mL) was added K2CO3 (5.5 g, 40.0 mmol), tetrakistriphenylphosphine Pd(0) (671 mg, 0.58 mmol) and 5-(5,5-dimethyl-1,3,2-dioxaborinane-2-yl)-1-methyl-1H-pyrazole (2.66 g, 13.71 mmol). The reaction mixture was heated to 80° C. in a sealed tube for 12 hours. The reaction mixture was partitioned between H2O and CHCl3. The pH of the aqueous phase was adjusted to ˜3 with 6N HCl and washed several times with CHCl3. The combined organic fractions were dried (Na2SO4), concentrated under vacuum and used directly without further purification (3.3 g, quant.): LC-MS (ES) m/z=289 (M+H)+.

1. customThe reaction mixture was partitioned between H2O and CHCl3
2. washwashed several times with CHCl3
3. dry with materialThe combined organic fractions were dried (Na2SO4)
4. concentrationconcentrated under vacuum
5. customused directly without further purification (3.3 g, quant.)