反应详情

温度

100 °C

The reaction mixture of tert-butyl piperidin-4-ylcarbamate (200 mg, 0.10 mmol), 2-bromopyridine (205 mg, 1.30 mmol), Pd2(dba)3 (18.0 mg, 0.02 mmol), Xantphos (35.0 mg, 0.06 mmol) and Cs2CO3 (490 mg, 1.50 mmol) was heated at 100° C. for 1 day. Additional 2-bromopyridine (205 mg, 1.30 mmol), Pd2(dba)3 (18.0 mg, 0.02 mmol), Xantphos (35.0 mg, 0.06 mmol), Cs2CO3 (490 mg, 1.50 mmol) were added to the reaction mixture, and heated at 100° C. for 1 day. The reaction mixture was cooled to room temperature, diluted with EtOAc and water. The separated aqueous layer was extracted with EtOAc, the combined organic layers were dried over Na2SO4, filtered, and concentrated in vacuo. The residue was purified by column chromatography (EtOAc) to give tert-butyl 1-(pyridin-2-yl)piperidin-4-ylcarbamate (86.8 mg, 31%) as a pale yellow solid. m/z=278.06 [M+1]+.

1. temperatureheated at 100° C. for 1 day
2. temperatureThe reaction mixture was cooled to room temperature
3. extractionThe separated aqueous layer was extracted with EtOAc
4. dry with materialthe combined organic layers were dried over Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by column chromatography (EtOAc)