反应详情

温度

0 °C

To a solution of 2-{2-[(4-nitrophenyl)amino]-3H-imidazo[4,5-b]pyridin-3-yl}ethanol (2.2 g) and triethylamine (10 mL) in THF (100 ml) was added methanesulfonyl chlorode (1.1 mL) at 0° C., and the mixture was stirred at 0° C. for 2 h. The mixture was poured into water and extracted with AcOEt. The organic layer was washed with brine, dried over Na2SO4, filtered and concentrated under reduced pressure. A mixture of the residue and potassium carbonate (3.1 g) in NMP (30 mL) was stirred at 100° C. overnight. After cooling to room temperature, the mixture was diluted with water. The formed crystals were collected by filtration to give the title compound (1.7 g).

1. extractionextracted with AcOEt
2. washThe organic layer was washed with brine
3. dry with materialdried over Na2SO4
4. filtrationfiltered
5. concentrationconcentrated under reduced pressure
6. additionA mixture of the residue and potassium carbonate (3.1 g) in NMP (30 mL)
7. stirringwas stirred at 100° C. overnight
8. temperatureAfter cooling to room temperature
9. additionthe mixture was diluted with water
10. filtrationThe formed crystals were collected by filtration