反应详情

温度

2.5 °C

2,2,7-trifluoro-2H-benzo[b][1,4]oxazin-3(4H)-one (2.5 g, 12.31 mmol) was dissolved in sulfuric acid (40 ml, 750 mmol). The reaction mixture was cooled to 0-5° C. Slowly nitric acid (1.761 ml, 39.7 mmol) was added dropwise and the temperature was maintained between 0-5° C. The reaction mixture was stirred for 30 min at this temperature. Then the reaction mixture was added dropwise to vigorously stirred cold water. A solid was formed, extraction with Dichloromethane. The combined extracts were dried over Na2SO4, and concentrated to yield 2.56 g of the title compound as brown solid.

1. temperaturethe temperature was maintained between 0-5° C
2. customA solid was formed
3. extractionextraction with Dichloromethane
4. dry with materialThe combined extracts were dried over Na2SO4
5. concentrationconcentrated