Model No.: 924-99-2
Ethyl 3-(Dimethylamino)acrylate CAS number is 924-99-2, which is the intermediate of the moxifloxacin. The synthesis method of Ethyl 3-(Dimethylamino)acrylate is as follows: (1) by DMF and ethoxy acetylene as raw materials by addition reaction, and reacted at 20℃for 20 days, the yield is 25%. (2) using tert-butoxy-2-dimethylaminomethane and ethyl acetate as raw materials at 170℃ for 20 hours, the yield is 88%; (3) with ethyl acrylate or diethyl malonate and KOH The monopotassium salt is prepared by reacting with DMF-dimethyl sulfate condensate salt, and the yield is up to 88%; (4) made of N,N-dimethylbenzyl acrylate as raw material, and zinc bromide is used as catalyst; The methicone was obtained as a solvent, and the yield was 29%.
The above experimental data shows that the method using DMF and ethoxy acetylene as raw materials is too long, the yield is low, and it is not suitable for industrialization. The method using N,N-dimethylbenzyl acrylate as a raw material is also too low in yield, and carbonitrile is used as a solvent, which is highly toxic. The method using tert-butoxy-2-dimethylaminomethane and ethyl acetate as a raw material has a high temperature and a long time, high raw material cost and high energy consumption. There is a technical solution that is more feasible. The general process is as follows:
1) adding 1.2:1 molar ratio, adding diethyl sulfate to DMF, controlling temperature at 80-90℃, holding for 2-5 hours, forming DMF-diethyl sulfate condensation salt solution;
2) mixing DMF-diethyl sulfate condensate solution with diethyl malonate, solvent and catalyst, heating to reflux and reacting for 3 to 10 hours, and then lowering to room temperature;
3) After the reaction is completed, the temperature is lowered to 10 to 20℃, filtered, and the filtrate is washed with water, and the layers are separated. The organic layer is collected, concentrated under reduced pressure, and then distilled under high vacuum under reduced pressure. The fraction collected at 80-85 ℃ / 5 mmHg is Ethyl 3-(Dimethylamino)acrylate CAS number is 924-99-2,
The yield and purity of this method are both at their best in the prior art. The preparation process is simple and easy, the reaction temperature is low, the time is short, the intermediate product does not need to be separated, energy saving and environmental protection, the production cost is low, the product quality is good, and the large-scale production is easy to be realized.
Thera. Category: Antibiotic
Cas No.: 924-99-2
Synonym:4-Dichloro-5-Fluorosbenzoylchloride;2,4-DICHLORO-5-FLUOROBENZOYL CHLORIDE;Benzoyl chloride,2,4-dichloro-5-fluoro-;2,4-Dichloro-5-fluorobenzoylchloride98%;2,4-Dichloro-5-fluorobenzoyl chloride 98%;2,4-DICHLORO-5-FLUOROBENZOYL CHLORIDE, 9 6%
Packing: Export worthy packing
lMaterial Safety Data Sheet: Available on request
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