反应详情

温度

110 °C

To a 350 mL sealed flask reactor was added methyl 4-(4-bromo-1-methyl-1H-pyrazol-5-yl)-2-thiophenecarboxylate (3.45 g, 11.46 mmol) [prepared according to the procedure of Example 156], trimethylboroxine (2.7 ml, 19.40 mmol), K2CO3 (4.75 g, 34.4 mmol) and Pd(dppf)Cl2 (599 mg, 1.17 mmol) in N,N-Dimethylformamide (DMF) (57 mL). The reaction was heated at 110° C. for 1 hour, cooled to room temperature and partitioned between CHCl3/H2O. The organic layer was separated, dried with Na2SO4, adsorbed onto silica and purified via column chromatography (0-30% EtOAc/Hexane) affording the title compound (2.07 g, 8.76 mmol, 76%): LC-MS (ES) m/z=251 (M+H)+.

1. customTo a 350 mL sealed flask reactor
2. customprepared
3. temperaturecooled to room temperature
4. custompartitioned between CHCl3/H2O
5. customThe organic layer was separated
6. dry with materialdried with Na2SO4
7. custompurified via column chromatography (0-30% EtOAc/Hexane)