反应详情

温度

80 °C

A mixture of tert-butyl 4-(6-(methoxycarbonyl)pyridin-3-yl)piperazine-1-carboxylate 49-3 (1.93 g, 6.01 mmol) and NaOH (530 mg, 13.26 mmol) in dioxane (15 mL) and H2O (15 mL) was stirred at 80° C. for 2 hours. Dioxane was removed by rotary evaporation and the resulting solution was acidified to pH around 4 by 1N HCl aqueous solution, followed by extraction with ethyl acetate (60 mL×3). The combined organic layers were washed with H2O and brine, dried over Na2SO4, and concentrated to dryness by rotary evaporation to afford 5-(4-(tert-butoxycarbonyl)piperazin-1-yl)picolinic acid 49-4 as a yellow solid. MS m/z 308.1 (M+1)

1. customDioxane was removed by rotary evaporation
2. extractionfollowed by extraction with ethyl acetate (60 mL×3)
3. washThe combined organic layers were washed with H2O and brine
4. dry with materialdried over Na2SO4
5. concentrationconcentrated to dryness by rotary evaporation