反应详情

温度

20 °C

To a solution of 1-benzyl-4-methyl-4-piperidinol obtained in Example 10-1 (3.34 g) in acetonitrile (19 mL) was added dropwise conc. sulfuric acid (16 mL) with cooling on an ice bath. The mixture was warmed to 20° C. and stirred for 15 hrs. After cooling, the reaction mixture was quenched by adding 3N potassium hydroxide solution, and the resulting solution (pH9) was extracted with ethyl acetate three times. The combined organic extracts were washed with brine, dried over MgSO4, and concentrated. The residual solid was triturated with ether to give the title compound as a white powder (3.55 g).

1. temperaturewith cooling on an ice bath
2. temperatureAfter cooling
3. customthe reaction mixture was quenched
4. additionby adding 3N potassium hydroxide solution
5. extractionthe resulting solution (pH9) was extracted with ethyl acetate three times
6. washThe combined organic extracts were washed with brine
7. dry with materialdried over MgSO4
8. concentrationconcentrated
9. customThe residual solid was triturated with ether