反应详情

A mixture of kojic acid (28.4 g, 0.20 mole), 120 mL of N,N-dimethylformamide, potassium carbonate powder (27.6 g, 0.20 mole), potassium iodide (1.66 g, 0.01 mole), and 1-bromopropane (24.6 g, 0.20 mole) is stirred for 15 minutes at ambient temperature then stirred at 90° C. for 3 hours. The reaction mixture is cooled, evaporated to dryness in vacuo and then portioned between water and chloroform. The aqueous layer is extracted with chloroform (3×100 mL) and ethyl acetate (6×100 mL). The combined organics were dried with sodium sulfate and passed through a pad of magnesol and silica gel eluting with ethyl acetate. The eluate is evaporated in vacuo and crystallized with hexane/ethyl acetate (2/1) to give an off-white solid, 22.60 g, (61%); MS (ES+): m/z 185.3 (M+H).

1. stirringthen stirred at 90° C. for 3 hours
2. temperatureThe reaction mixture is cooled
3. customevaporated to dryness in vacuo
4. extractionThe aqueous layer is extracted with chloroform (3×100 mL) and ethyl acetate (6×100 mL)
5. dry with materialThe combined organics were dried with sodium sulfate
6. customThe eluate is evaporated in vacuo
7. customcrystallized with hexane/ethyl acetate (2/1)
8. customto give an off-white solid, 22.60 g, (61%)