反应详情

To a clean, dry 100 mL round bottom flask is added 3-hydroxy-5-nitrobenzoic acid (1 g, 5.5 mmole, 1 eq) followed by 10 mL methanol and 2 mL of concentrated sulfuric acid. The exothermic reaction mixture reached 60° C. prior to cooling to room temperature. The reaction mixture was stirred for 18 h prior to partitioning between ethyl acetate and water. After extraction, the organic layer was dried over magnesium sulfate, filtered and evaporated. A white solid product was obtained (1 g, 100%). Calc'd for C8H7NO5; m/z (M+H+)=198; found 198.

1. customTo a clean, dry 100 mL round bottom flask
2. customreached 60° C.
3. customto partitioning between ethyl acetate and water
4. extractionAfter extraction
5. dry with materialthe organic layer was dried over magnesium sulfate
6. filtrationfiltered
7. customevaporated
8. customA white solid product was obtained (1 g, 100%)