反应详情

A solution of 4-(4-Bromo-phenyl)-4-(4-hydroxy-phenyl)piperidine-1-carboxylic acid tert-butyl ester (100 mg, 0.23 mmol), 2-bromoethyl methylether (200 ul) and potassium carbonate (64 mg, 0.46 mmol) in dimethylformamide (2 ml) was heated in a CEM Explorer™ microwave to 50° C. for 30 minutes using 50 watts power. The reaction was poured into sodium hydroxide (2N, 4 ml), stirred for 5 minutes then extracted into ethyl acetate (2×30 ml). The combined organic liquors were dried (MgSO4), concentrated and the residue was purified by column chromatography (SiO2), eluting with ethyl acetate/petrol (25:75) gradient to (50:50) to afford the title compound (82 mg). LCMS: (PS-A2) Rt 4.00 [M+H]+ 490.

1. extractionthen extracted into ethyl acetate (2×30 ml)
2. dry with materialThe combined organic liquors were dried (MgSO4)
3. concentrationconcentrated
4. customthe residue was purified by column chromatography (SiO2)
5. washeluting with ethyl acetate/petrol (25:75) gradient to (50:50)