反应详情

2.78 g of 2-mercaptopyrimidine were added to a solution of 1.95 g of 85% potassium hydroxide and 9.03 g of N-[4-(4-piperidinomethyl-2-pyridyloxy)-cis-2-butenyl]-4-chlorobutyramide (prepared as described in Preparation 2) in 140 ml of methanol, and the resulting mixture was heated under reflux for 15 hours. At the end of this time, the reaction mixture was cooled, and the solvent was removed by distillation under reduced pressure. The resulting residue 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 9:1 by volume mixture of ethyl acetate and methanol as the eluent, to give 10.1 g (yield 92%) of the title compound as an oil.

1. temperaturethe resulting mixture was heated
2. temperatureunder reflux for 15 hours
3. temperatureAt the end of this time, the reaction mixture was cooled
4. customthe solvent was removed by distillation under reduced pressure
5. additionThe resulting residue was mixed with water
6. extractionthe aqueous mixture was extracted with ethyl acetate
7. concentrationThe extract was concentrated by evaporation under reduced pressure
8. customthe concentrate was purified by column chromatography through silica gel
9. additionby volume mixture of ethyl acetate and methanol as the eluent