反应详情

In a 100 ml three-necked flask equipped with a mechanical stirrer, dropping funnel, reflux condenser, and a nitogen-inlet tube, 9.9 gm (57 mmol) of above-mentioned 3-(1-ethoxyethoxy)-3-methyl-butane-2-one, 2.3 gm (57 mmol) of 60% sodium hydride, 5.0 gm (25 mmol) of dimethylterephthalate and 50 ml of anhydrous tetrahydrofuran were mixed with stirring under nitrogen stream, and the refluxing under heat was continued for 7 hours. After cooling the reaction mixture, 30 ml of 2N hydrochloric acid was added and the mixture was extracted with chloroform. The extract was dried over anhydrous sodium sulfate and the solvent was removed by evaporation. The reaction mixture was stirred at room temperature while adding 30 ml of methnol with ten drops of 2N hydrochloric acid. A mixed solvent of acetone-chloroform was added to the crude product, and recrystallization afforded 4.1 gm of the title compound as pale yellow crystals (yield: 48%).

1. customIn a 100 ml three-necked flask equipped with a mechanical stirrer
2. temperaturereflux condenser, and a nitogen-inlet tube
3. temperaturethe refluxing under heat
4. additionwas added
5. extractionthe mixture was extracted with chloroform
6. dry with materialThe extract was dried over anhydrous sodium sulfate
7. customthe solvent was removed by evaporation
8. stirringThe reaction mixture was stirred at room temperature
9. additionwhile adding 30 ml of methnol with ten drops of 2N hydrochloric acid
10. additionA mixed solvent of acetone-chloroform was added to the crude product, and recrystallization