反应详情

温度

50 °C

Dissolve a solution of 4-(3-chloro-5-ethoxycarbonyl-pyridin-2-yl)-piperazine-1-carboxylic acid tert-butyl ester (7.78 g, 0.021 mol) in dioxane, and then add a solution of 4M HCl/dioxane (12 mL). Stir at 50° C. for 2 h, and then add additional 4M HCl/dioxane (5 mL) and stir for an additional 1 h. Cool the mixture in ice, collect the precipitate and wash with ether. Prepare the freebase by partitioning between EtOAc and 10% NaOH solution. Dry the organic layer (Na2SO4) and concentrate under reduced pressure to give the title compound.

1. stirringstir for an additional 1 h
2. temperatureCool the mixture in ice
3. customcollect the precipitate
4. washwash with ether
5. customPrepare the freebase
6. customby partitioning between EtOAc and 10% NaOH solution
7. dry with materialDry the organic layer (Na2SO4)
8. concentrationconcentrate under reduced pressure