反应详情

温度

100 °C

To a solution of 2-amino-4-trifluoromethyl-5-iodo-benzoic acid methyl ester (750 mg, 2.17 mmol) in dioxane (15 mL) were added 1-benzyloxy-5-tributylstannanyl-1H-pyrazole (1.24 g, 2.60 mmol) and Pd(dppf)2Cl2 (177 mg, 0.217 mmol) and the resulting mixture was stirred at 100° C. for 16 h. An additional portion of catalyst (0.1 equiv) was added and the mixture was stirred at 100° C. for an additional 24 h. The solvent was removed in vacuo to afford a dark oil. The crude product was purified by flash chromatography (silica gel, EtOAc/hexanes (0:100 to 50:50)) to provide the title compound as an off-white solid (263 mg, 31%). ES-MS: m/z 392.3 [M+H]+, rt 6.48 min.

1. stirringthe mixture was stirred at 100° C. for an additional 24 h
2. customThe solvent was removed in vacuo
3. customto afford a dark oil
4. customThe crude product was purified by flash chromatography (silica gel, EtOAc/hexanes (0:100 to 50:50))