反应详情

A mixed solution of 0.73 g of 1-cyclopropylethylamine hydrochloride and 0.91 g of triethylamine in 12 ml of acetonitrile was stirred at room temperature for one hour. Then, to the mixed solution, 0.53 g of crude crystals of methyl (E)-3-(6-chloro-4-oxo-4H-benzo[d][1,3]oxazin-2-yl)acrylate were added at room temperature and reacted for 3 hours at room temperature. To the reaction liquid, water was added, and then ethyl acetate was added for extraction. The organic layer was washed with a saturated sodium chloride aqueous solution and dried over anhydrous sodium sulfate. The solvent was distilled off under reduced pressed, and the residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=9/1 to 8/2) to obtain 0.22 g of the desired product having a slightly yellow color (melting point: 154.4° C.).

1. customreacted for 3 hours at room temperature
2. additionwas added
3. washThe organic layer was washed with a saturated sodium chloride aqueous solution
4. dry with materialdried over anhydrous sodium sulfate
5. distillationThe solvent was distilled off
6. customthe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=9/1 to 8/2)