反应详情

温度

70 °C

11.1 g (1.5 eq) tert-butyl-2-bromoethylcarbamate dissolved in 65 ml THF and 9.19 g (2 eq) potassium carbonate were added to a solution of 7 g (1 eq) N,N-dimethyl-4-(thiophen-2-yl)piperidin-4-amine in 40 ml THF. The reaction mixture was heated for 6 h at 70° C. The reaction course was monitored by thin-layer chromatography (20% MeOH/CHCl3). Once the conversion was complete, the solvent was distilled off completely, the residue mixed with 200 ml water and the aqueous phase extracted with 20% IPA/CHCl3. The combined organic phases were dried over Na2SO4. Following removal of the solvent under reduced pressure, the residue was purified by column chromatography (silica gel; 10% MeOH/CHCl3). 9 g (76%) of product were obtained in the form of an oil.

1. distillationthe solvent was distilled off completely
2. additionthe residue mixed with 200 ml water
3. extractionthe aqueous phase extracted with 20% IPA/CHCl3
4. dry with materialThe combined organic phases were dried over Na2SO4
5. customremoval of the solvent under reduced pressure
6. customthe residue was purified by column chromatography (silica gel; 10% MeOH/CHCl3)