反应详情

4-Hydroxy-4-phenyl-piperidine-1-carboxylic acid tert-butyl ester (0.5 g, 1.8 mmol) was dissolved in dry THF (15 mL) and sodium hydride (60% disp. in mineral oil; 0.076 g, 1.9 mmol) added and the mixture stirred for 1 hour. Methyl iodide (0.16 mL; 2.7 mmol) was then added and the mixture stirred overnight. Brine was added and the product extracted into ethyl acetate, dried over sodium sulphate, filtered and the solvent removed by evaporation. The residue was purified by flash chromatography on silica eluting with 0-10% ethyl acetate/hexane. The fractions containing the desired product were concentrated under vacuum to give the title compound as a clear colourless oil (0.35 g).

1. stirringthe mixture stirred overnight
2. extractionthe product extracted into ethyl acetate
3. dry with materialdried over sodium sulphate
4. filtrationfiltered
5. customthe solvent removed by evaporation
6. customThe residue was purified by flash chromatography on silica eluting with 0-10% ethyl acetate/hexane
7. additionThe fractions containing the desired product
8. concentrationwere concentrated under vacuum