反应详情

To a solution of 3-[4-(6-fluoro-benzothiazol-2-ylamino)-phenyl]-isoxazole-5-carboxylic acid amide (3.54 g; 10 mmol) in dioxane (25 ml), was added Lawesson's reagent (4.11 g; 10 mmol) and the resulting reaction mixture was refluxed for 45 min. The pH of the reaction mixture was adjusted to near neutral, the solvent was removed and the residue was diluted with water (20 ml) and extracted with EtOAc (3×30 ml). The EtOAc layer was washed with water (3×10 ml) followed by brine (10 ml), and dried over anhydrous Na2SO4. The solvent was removed, and the residue was triturated with dichloromethane, filtered and dried to afford 3.0 g (80%) of the title compound. Mass (ES−), 369 (M−1); IR (KBr): 3282 (br), 3142 (br), 1651, 1608, 1588, 1555, 1441 (br); 1H NMR (DMSO-d6) δ: 7.18 (m, 1H), 7.58 (s, 1H), 7.65 (m, 1H), 7.77 (m, 1H), 7.88-7.94 (br, 4H), 7.97, 10.33 (2×br, 2H), 10.79 (s, 1H).

1. customthe resulting reaction mixture
2. temperaturewas refluxed for 45 min
3. customthe solvent was removed
4. additionthe residue was diluted with water (20 ml)
5. extractionextracted with EtOAc (3×30 ml)
6. washThe EtOAc layer was washed with water (3×10 ml)
7. dry with materialdried over anhydrous Na2SO4
8. customThe solvent was removed
9. customthe residue was triturated with dichloromethane
10. filtrationfiltered
11. customdried