反应详情

温度

100 °C

A mixture of 19 g of 2-chloro-6-(2,2,2-trifluoroethoxy)pyridine (b.p. 80° C./16 mm Hg, prepared by reaction of 2,6-dichloropyridine with 2,2,2-trifluoroethanolate of sodium), 14.87 g of 4-formamidopiperidine (m.p. 116° to 118° C., prepared by hydrogenation of 4-formamido-1-benzylpiperidine in the presence of palladium on charcoal), 17.27 g of anhydrous potassium carbonate, 5.67 g of copper in powder form in 110 ml of sulfolane is heated to 100° C. with stirring for 50 hours, then the sulfolane is distilled, the residue is taken up with water and the suspension thus obtained is extracted with methylene chloride. The organic phase is washed with water, it is dried over anhydrous sodium sulfate and evaporated to dryness. The residue, firstly crystallised in an 84/16 by volume mixture of water/ethanol and afterwards in diisopropylic ether, gives 9 g of 4-acetamido-1-[6-(2,2,2-trifluoro)ethoxy-2-pyridyl] piperidine; m.p. 92° to 95° C.

1. distillationthe sulfolane is distilled
2. customthe suspension thus obtained
3. extractionis extracted with methylene chloride
4. washThe organic phase is washed with water, it
5. dry with materialis dried over anhydrous sodium sulfate
6. customevaporated to dryness
7. customThe residue, firstly crystallised in an 84/16 by volume mixture of water/ethanol and afterwards in diisopropylic ether