反应详情

温度

70 °C

60% oily sodium hydride (256 mg, 6.4 mmol) was added to a solution of 2-hydroxy-7-hydroxymethyl-4-isopropyl-2,4,6-cycloheptatrien-1-one (1.13 g, 5.82 mmol) in dimethylformamide (5 ml) with stirring. Then, ethyl iodide (0.7 ml, 8.75 mmol) was added and the reaction mixture was heated at 70° C. for 3 hours. The reaction solution was diluted with dichloromethane, washed with water, and dried over sodium sulfate. After the solvent was distilled off under reduced pressure, the residue was purified by silica gel column chromatography [eluent:hexane/ethyl acetate (2:3)] to give 485 mg of 2-ethoxy-7-hydroxymethyl 4-isopropyl-2,4,6-cycloheptatrien-1-one as a pale yellow amorphous powder (yield: 76%).

1. washwashed with water
2. dry with materialdried over sodium sulfate
3. distillationAfter the solvent was distilled off under reduced pressure
4. customthe residue was purified by silica gel column chromatography [eluent:hexane/ethyl acetate (2:3)]