反应详情

温度

100 °C

To a solution of 1-benzyl-4-methyl-piperidin-4-ol (0.4 g, 1.95 mmol) in bromobenzene (1.2 mL) was added aluminium trichloride (0.39 g, 2.9 mmol). The mixture was then heated to 100° C. for 14 hours and left standing at room temperature for 48 hours. Aqueous sodium hydroxide (1 N, 30 mL) was added and the products extracted into ethyl acetate, dried over magnesium sulphate, filtered and the solvent removed by evaporation under vacuum. The residue was purified by flash chromatography on silica eluting with 0-25% ethyl acetate/hexane. The fractions containing the desired product were concentrated under vacuum to give the title compound as a brown oil (0.5 g). LCMS m/z 344.5 [M+H]+. R.T.=3.13 min (Analytical Method 4).

1. waitleft
2. extractionthe products extracted into ethyl acetate
3. dry with materialdried over magnesium sulphate
4. filtrationfiltered
5. customthe solvent removed by evaporation under vacuum
6. customThe residue was purified by flash chromatography on silica eluting with 0-25% ethyl acetate/hexane
7. additionThe fractions containing the desired product
8. concentrationwere concentrated under vacuum