反应详情

温度

-20 °C

5-Amino-2-(2-methylpyridin-3-yloxy)pyridine (D9, 60.3 g, 0.3 mole) in dry CH2Cl2 (2.5L) was cooled to −20° C. under argon. Triethylamine (46 ml, 0.33 mole) was added, followed dropwise by phenyl chloroformate (41 ml, 0.33 mole) and the mixture was stirred at −20° C. for 1 hour. After warming to ambient temperature, the mixture was washed with dil. aq. NaHCO3, dried (Na2SO4) and evaporated in vacuo. The residue was recrystallised from ethyl acetate/60-80° petroleum ether to afford the title compound (53.7 g, 56%) as a pink solid.

1. temperatureAfter warming to ambient temperature
2. washthe mixture was washed with dil. aq. NaHCO3
3. dry with materialdried (Na2SO4)
4. customevaporated in vacuo
5. customThe residue was recrystallised from ethyl acetate/60-80° petroleum ether