反应详情

温度

69.5 °C

To a solution of N-[(3-benzyloxy-5-bromo-phenyl)carbamothioyl]benzamide (648 g, 1.47 mol) in THF (12 L) was added NaOH solution (300 g, 7.5 mol in 3 L H2O) at rt. The reaction mixture was heated up to 69 to 70° C. overnight. After completion of reaction (by TLC), the THF layer was decanted off and the aqueous layer extracted with EtOAc (3×2 L). The combined organic layer (THF+EtOAc) was washed with brine, dried over anhydrous Na2SO4, filtered and concentrated under reduced pressure. The crude residue was treated with mixture of Et2O and hexane (5:95, 3.0 L), filtered, washed with hexane and dried under high vacuum to obtain the desired product (387 g, 78%).

1. customAfter completion of reaction (by TLC)
2. customthe THF layer was decanted off
3. extractionthe aqueous layer extracted with EtOAc (3×2 L)
4. washThe combined organic layer (THF+EtOAc) was washed with brine
5. dry with materialdried over anhydrous Na2SO4
6. filtrationfiltered
7. concentrationconcentrated under reduced pressure
8. additionThe crude residue was treated with mixture of Et2O and hexane (5:95, 3.0 L)
9. filtrationfiltered
10. washwashed with hexane
11. customdried under high vacuum