反应详情

温度

105 °C

A mixture of 2-methyl-benzooxazol-6-ol (8.41 g, 56 mmol), 5-nitro-1,3-dioxo-1,3-dihydro-isoindol-2-yl)-acetic acid ethyl ester (17.23 g, 62 mmol), potassium carbonate (9.36 g, 67.7 mmol), and dimethylacetamide (120 mL) was stirred at 105° C. for twenty hours before it was cooled to room temperature and partitioned between chloroform and water. The organic layer was dried over anhydrous sodium sulfate, concentrated in vacuo and the residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and dichloromethane to give the title compound as a yellow solid (9.18 g): MS: (+) m/z 381.27 (M+1).

1. temperaturewas cooled to room temperature
2. custompartitioned between chloroform and water
3. dry with materialThe organic layer was dried over anhydrous sodium sulfate
4. concentrationconcentrated in vacuo
5. customthe residue was purified by flash column chromatography on silica gel with a gradient of ethyl acetate and dichloromethane