反应详情

温度

150 °C

To a solution of methanesulfonic acid (R)-6-benzyloxy-2,3-dihydrobenzo[1,4]dioxin-2-ylmethyl ester (129 mg, 0.368 mmol) and (R*)-3-(piperidin-3-yl)phenol.HBr (100 mg, 0.387 mmol) in acetonitrile was added solid KI (40 mg) and NaHCO3 (98 mg 1.162 mmol). The mixture was heated under microwave irradiation at 150° C. for 1 h. Solid material was filtered and the solvent was evaporated under reduced pressure. The residue was dissolved to DCM and washed twice with water and brine. The organic phase was dried (Na2SO4), and evaporated in vacuo. The residue was purified by flash column chromatography (EtOAc/heptane) to give the desired product (66.2 mg).

1. filtrationSolid material was filtered
2. customthe solvent was evaporated under reduced pressure
3. dissolutionThe residue was dissolved to DCM
4. washwashed twice with water and brine
5. dry with materialThe organic phase was dried (Na2SO4)
6. customevaporated in vacuo
7. customThe residue was purified by flash column chromatography (EtOAc/heptane)