反应详情

温度

65 °C

A solution of Pd(OAc)2 (6 mg, 0.025 mmol) and rac-BINAP (23 mg, 0.037 mmol) in THF (2.5 mL) was stirred under nitrogen for 10 min. Cs2CO3 (95 mg, 0.29 mmol), 4-methyl-2-(5-trifluoromethanesulfonyloxy-4′-trifluoromethyl-biphenyl-3-yl)-pentanoic acid methyl ester (100 mg, 0.21 mmol) and indoline (0.028 mL, 0.25 mmol) were added and the reaction mixture was stirred under nitrogen at 65° C. for 48 h. The solution was then partitioned between EtOAc (10 mL) and H2O (10 mL). The aqueous layer was extracted with EtOAc (2×10 mL). The organic layers were washed with brine, dried (MgSO4) and concentrated to yield an oil. The residue was purified by flash chromatography (0 to 10% EtOAc in petroleum ether) to give the title compound. The resulting oil was used crude in the next step.

1. customThe solution was then partitioned between EtOAc (10 mL) and H2O (10 mL)
2. extractionThe aqueous layer was extracted with EtOAc (2×10 mL)
3. washThe organic layers were washed with brine
4. dry with materialdried (MgSO4)
5. concentrationconcentrated
6. customto yield an oil
7. customThe residue was purified by flash chromatography (0 to 10% EtOAc in petroleum ether)