反应详情

7-Hydroxy-4-methylcoumarin-3-acetic acid (1) (1 gm, 4.3 mmol) was suspended in anhydrous ethanol (15 mL), concentrated sulfuric acid (1.5 mL) was added and the mixture was heated at reflux for 1 hour. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (100 mL), washed with 5% NaHCO3 (5×50 mL), water (2×50 mL), saturated NaCl (2×50 mL) dried with sodium sulfate, filtered and the filtrate was evaporated under reduced pressure to give 1.04 gm (4.0 mmol, 92% yield of 2 as a white solid. 1H NMR (CDCl3 /DMSO-d6): 1.19 (3H,t), 2.29 (3H,s), 3.57 (2H,s), 4.06 (2H,q), 6.65 (1H,d), 6.73 (1H,dd), 7.44 (1H,d).

1. temperaturethe mixture was heated
2. temperatureat reflux for 1 hour
3. washwashed with 5% NaHCO3 (5×50 mL), water (2×50 mL), saturated NaCl (2×50 mL)
4. dry with materialdried with sodium sulfate
5. filtrationfiltered
6. customthe filtrate was evaporated under reduced pressure