反应详情

14 g (0.6 mol) of 100% pure sodium hydride and 54 g (0.6 mol) of dimethyl carbonate in 225 ml of absolute diethyl ether are initially taken under nitrogen. 72 g (0.3 mol) of 2-(2-methylbenzyloxy)-acetophenone, dissolved in 300 ml of absolute ether, are added dropwise at 20°-35° C. and the mixture is refluxed for 5 h. At 10° C., first 45 ml of methanol and then 100 ml of H2O are slowly added dropwise. The pH is then brought to 7 with dilute hydrochloric acid. The organic phase is washed several times with H2O, dried over sodium sulfate and evaporated down. The product is obtained in quantitative yield as crystals (mp.=38°-42° C.).

1. additionare added dropwise at 20°-35° C.
2. temperaturethe mixture is refluxed for 5 h
3. washThe organic phase is washed several times with H2O
4. dry with materialdried over sodium sulfate
5. customevaporated down