反应详情

温度

40 °C

Method C—Step a To a mixture of 5-Bromo-2-chlorobenzoic acid (5.00 g, 21.23 mmol) in DMF (40 mL), HATU (8.48 g, 22.29 mmol) and triethylamine (2.97 mL, 21.44 mmol) were added. After 30 min stirring at room temperature 4-nitro-pyridin-3ylamine (2.36 g, 16.99 mmol) was added, the reaction mixture stirred at 40° C. overnight and solvent removed. The crude was then diluted with EtOAc (40 mL) and washed first with saturated Na2CO3 solution (6×30 mL) then 1N HCl (3×30 mL). The organic layer was dried over Na2SO4, filtered and left standing. The precipitate obtained was filtered to get 4.75 g of the title compound (63%).

1. additionwere added
2. additionwas added
3. customsolvent removed
4. additionThe crude was then diluted with EtOAc (40 mL)
5. washwashed first with saturated Na2CO3 solution (6×30 mL)
6. dry with materialThe organic layer was dried over Na2SO4
7. filtrationfiltered
8. waitleft
9. customThe precipitate obtained
10. filtrationwas filtered