反应详情

To a mixture of 2-trifluoromethoxy-phenyl-boronic acid (0.307 g, 2.24 mmol, 1.5 eq.), ligand TFP (0.069 g, 0.298 mmol, 0.2 eq.), Pd2(dba)3 (0.154 g, 0.149 mmol, 0.1 eq.), copper (I) thiophene-2-carboxylate (0.426 g, 2.24 mmol, 1.5 eq.) was added a solution of p-tolylsulfanylcarbonyl-piperidine-1-carboxylic acid tert-butyl ester (0.479 g, 1.49 mmol, 1 eq.) in 15 mL of DME while purging with N2 at room temperature. After 18 h stirring at room temperature, the reaction mixture was diluted with ethyl acetate and filtered through celite. The filtrate was concentrated to give an oil. This oil was purified by silica gel column chromatography (10% ethyl acetate/heptane) to give the title compound as a white solid (0.5 g, 86%). Exact mass calculated for C18H23F3N1O4 374.2. MS (ESI) m/z 274.3 [(M-100)H]+.

1. customwhile purging with N2 at room temperature
2. additionthe reaction mixture was diluted with ethyl acetate
3. filtrationfiltered through celite
4. concentrationThe filtrate was concentrated
5. customto give an oil
6. customThis oil was purified by silica gel column chromatography (10% ethyl acetate/heptane)