反应详情

1.68 ml of triethylamine were added to a solution of 3.00 g of 3-(4-piperidinomethyl-2-pyridyloxy)propylamine in 60 ml of ethyl acetate, and the resulting mixture was cooled with ice, after which 0.96 ml of 2-chloroacetyl chloride was added. The reaction mixture was then stirred at room temperature for 1 hour, after which it was mixed with water and the aqueous mixture was extracted with ethyl acetate. The extract was concentrated by evaporation under reduced pressure, and the concentrate was purified by column chromatography through silica gel, using a 1:9 by volume mixture of methanol and ethyl acetate as the eluent, to give 3.40 g (yield 87%) of the title compound as an oil.

1. temperaturethe resulting mixture was cooled with ice
2. extractionthe aqueous mixture was extracted with ethyl acetate
3. concentrationThe extract was concentrated by evaporation under reduced pressure
4. customthe concentrate was purified by column chromatography through silica gel
5. additionby volume mixture of methanol and ethyl acetate as the eluent