反应详情

温度

70 °C

To a solution of N-(2,6-dibromopyridin-4-ylcarbamothioyl)benzamide (14.50 g, 34.93 mmol) in a mixture of THF (600 mL) and MeOH (200 mL) was added a solution of NaOH (7.0 g, 174.65 mmol) dissolved in 200 mL of water. The mixture was heated to 70° C. for 16-22 h. After reaction, the solvent wad distilled under reduced pressure, water added and extracted with EtOAc (3×500 mL). The combined organics were washed with brine, dried (Na2SO4), filtered and concentrated under reduced pressure. The residue thus obtained was treated with 20% EtOAc-hexane and finally filtered to obtain the desired product as an off-white solid (9.0 g, 83%).

1. customAfter reaction
2. distillationthe solvent wad distilled under reduced pressure, water
3. additionadded
4. extractionextracted with EtOAc (3×500 mL)
5. washThe combined organics were washed with brine
6. dry with materialdried (Na2SO4)
7. filtrationfiltered
8. concentrationconcentrated under reduced pressure
9. customThe residue thus obtained
10. filtrationfinally filtered