反应详情

温度

62.5 °C

To a solution of 1-benzoyl-3-(2,6-dibromo-pyridin-4-yl)-thiourea (1.0 g, 2.14 mmol) in THF (50 mL) was added NaOH solution (0.48 in 20 mL H2O) at room temperature. The reaction mixture was heated up to 60-65° C. overnight. After completion of reaction (TLC monitoring) THF was distilled off followed by addition of water, and extraction with ethyl acetate (2×50 mL). The combined organic layers were dried over anhydrous Na2SO4, filtered and evaporated to dryness under reduced pressure. The crude residue was washed with mixture of ethyl acetate:hexane (30:70) and dried under high vacuum to get the desired product as a white solid (0.58 g, 78%).

1. distillationwas distilled off
2. additionfollowed by addition of water, and extraction with ethyl acetate (2×50 mL)
3. dry with materialThe combined organic layers were dried over anhydrous Na2SO4
4. filtrationfiltered
5. customevaporated to dryness under reduced pressure
6. washThe crude residue was washed with mixture of ethyl acetate:hexane (30:70)
7. customdried under high vacuum