反应详情

温度

80 °C

A mixture of trifluoromethanesulfonic acid 3-{(R*)-1-[(S)-1-(2,3-dihydrobenzo[1,4]dioxin-2-yl)methyl]-piperidin-3-yl}phenyl ester (51 mg, 0.11 mmol), tributyltin cyanide (142 mg, 0.45 mmol) and tetrakis(triphenylphosphine)palladium (189 mg, 0.164 mmol) in 1,2-dichloroethane (15 ml) was heated in a microwave reactor at 80° C. for 80 h. The solid precipitate was filtered off and the mixture was evaporated to dryness. The residue was redissolved in DCM, filtered and washed two times with 1 M HCl. The combined organic phases were washed with brine, dried (Na2SO4) and evaporated to dryness. The crude product was purified by flash chromatography first using gradient of DCM and MeOH and then using gradient of heptane and EtOAc as eluent to give 2.8 mg of the title compound.

1. filtrationThe solid precipitate was filtered off
2. customthe mixture was evaporated to dryness
3. dissolutionThe residue was redissolved in DCM
4. filtrationfiltered
5. washwashed two times with 1 M HCl
6. washThe combined organic phases were washed with brine
7. dry with materialdried (Na2SO4)
8. customevaporated to dryness
9. customThe crude product was purified by flash chromatography