反应详情

Under vigorously agitation, 39.0 g of ethyl 2-oxocyclopentane carboxylate was added to 105.6 g (purity of 98%) of ground anhydrous potassium carbonate, and after stirring for several minutes, to the mixture was added 100 ml of acetone. The reaction mixture was further stirred for about 15 minutes, then thereto was dropwise added 34.35 ml (purity of 98%) of p-methylbenzyl bromide. Upon the completion of the addition, the reaction mixture was heated for reflux for 4 hours. The reaction mixture was filtered under the reduced pressure, and the filter cake was washed with diethyl ether until its color was purely white. Pale yellow filtrate was collected and dried over anhydrous magnesium sulfate, then the solvent was removed. The residue was distilled under reduced pressure, and 53.57 g of colorless liquid as a distillate cut of 144-146° C./100 Pa was collected. Yield: 82.4%. MS: m/e 260(M+′), 242, 232(M+′—CH2CH2), 215(M+′—OCH2CH3), 187(M+′—CO2CH2CH3), 171, 155(M+″—C8H9) 127, 105(base), 77.

1. stirringThe reaction mixture was further stirred for about 15 minutes
2. additionUpon the completion of the addition
3. temperaturethe reaction mixture was heated
4. temperaturefor reflux for 4 hours
5. filtrationThe reaction mixture was filtered under the reduced pressure
6. washthe filter cake was washed with diethyl ether until its color
7. customPale yellow filtrate was collected
8. dry with materialdried over anhydrous magnesium sulfate
9. customthe solvent was removed
10. distillationThe residue was distilled under reduced pressure, and 53.57 g of colorless liquid as a distillate cut of 144-146° C./100 Pa
11. customwas collected