反应详情

A solution of 3.00 g (17.96 mmol) of 3-bromo-2,2-dimethyl-propan-1-ol, 17.78 ml (179.59 mmol) of piperidine, 2.48 g (17.96 mmol) of K2CO3 and 2.69 g (17.96 mmol) of potassium iodide in 20 ml of DMA were stirred at 70° C. for 20 h. After filtration and evaporation of the solvents, the crude product was dissolved in diluted aqueous HCl solution and washed with EtOAc (3×). The aqueous phase was basified with KHCO3 and some drops of 1N NaOH and extracted with EtOAc (3×). The organic phase was dried (Na2SO4) and evaporated to give 0.57 g (18%) of the title compound as yellow liquid. MS: 172.0 (MH+).

1. filtrationAfter filtration and evaporation of the solvents
2. dissolutionthe crude product was dissolved in diluted aqueous HCl solution
3. washwashed with EtOAc (3×)
4. extractionsome drops of 1N NaOH and extracted with EtOAc (3×)
5. dry with materialThe organic phase was dried (Na2SO4)
6. customevaporated