反应详情

温度

75 °C

To a 16 ml vial was added tert-butyl 4-(1-mercaptoethyl)piperidine-1-carboxylate (500 mg, 2.04 mmol), 2-bromo-6-(trifluoromethyl)pyridine (460 mg, 2.04 mmol), Pd(dppf)Cl2 (42 mg, 0.051 mmol) and Cs2CO3 (996 mg, 3.06 mmol) and 4 ml toluene. The vial was flushed with nitrogen, sealed and heated at 75° C. for 36 hours. After cooling to room temperature, the reaction mixture was diluted with 30 ml ether, and washed with 30 ml water. The organics were dried over sodium sulfate, filtered and concentrated. The residue was purified on silica gel column eluted with 1:9 to 1:4 ethyl acetate/hexane to give 750 mg desired product was light yellow oil.

1. customThe vial was flushed with nitrogen
2. customsealed
3. temperatureAfter cooling to room temperature
4. additionthe reaction mixture was diluted with 30 ml ether
5. washwashed with 30 ml water
6. dry with materialThe organics were dried over sodium sulfate
7. filtrationfiltered
8. concentrationconcentrated
9. customThe residue was purified on silica gel column
10. washeluted with 1:9 to 1:4 ethyl acetate/hexane