反应详情

温度

80 °C

First, 7-hydroxy-2,4-dimethyl-2H-1,4-benzoxazine-3 (4H)-thione (0.2 g) and 3-chloro-4,5-difluorotrifluoromethylbenzene (0.3 g) were dissolved in DMSO (5 ml), potassium carbonate (0.2 g) was added thereto, and the mixture was stirred at 80° C. for one hr. Water (10 ml) was added thereto to terminate the reaction, and the reaction mixture was extracted with ethyl acetate (20 ml×2), washed with water and a saturated saline solution and dried over anhydrous magnesium sulfate. The solvent was distilled off in vacuo, and the residue was purified by silica gel chromatography (developing solvent: n-hexane/ethyl acetate=5/1) to prepare the title compound (0.2 g) as a colorless crystal.

1. customto terminate
2. customthe reaction
3. extractionthe reaction mixture was extracted with ethyl acetate (20 ml×2)
4. washwashed with water
5. dry with materiala saturated saline solution and dried over anhydrous magnesium sulfate
6. distillationThe solvent was distilled off in vacuo
7. customthe residue was purified by silica gel chromatography (developing solvent: n-hexane/ethyl acetate=5/1)
8. customto prepare the title compound (0.2 g) as a colorless crystal