Ethyl 2-phenylacetoace

Purpose 2-Phenylacetoacetate ethyl ester, also known as α- Ethyl phenylacetoacetate is an important pharmaceutical and chemical raw material, mainly used in the synthesis of intermediates that are indispensable for the fourth and fifth generation of new cephalosporin antibiotics. The application of 2-phenylacetoacetate ethyl ester as an organic ester can be used as a pharmaceutical intermediate. Preparation (1) Firstly, prepare a mixture of ethyl acetoacetate and toluene in a certain proportion, and then continuously inject the mixture and iodobenzene into a microchannel reactor using a metering pump at a certain proportion of flow rate. Control the outlet temperature of the reactor to 5-10 ℃; Then mix and layer the prepared saturated salt water continuously with the reaction solution, with the lower Chemicalbook layer as the reaction solution and the upper layer of salt water. (2) Under normal pressure, slowly raise the temperature of the washed reaction solution. When the bottom temperature of the reactor reaches 55 ℃, toluene begins to evaporate until the temperature of the reactor reaches 100 ℃ (ensuring complete solvent evaporation), stop heating, cool and collect the distilled solvent; (3) After recovering the solvent, perform vacuum distillation under a vacuum degree of -0.1MPa, slowly raise the temperature. When the kettle temperature is 85-90 ℃, control the reflux ratio to 4, and start to steam out the finished product. When the kettle temperature rises to 120 ℃, stop heating, and turn off the vacuum pump to obtain qualified finished product 2-phenylacetoacetate ethyl ester, and measure its chromatographic content.