Preparation method for edaravone
A technology of edaravone and protonic acid, which is applied in the field of preparation of brain protective agent edaravone, can solve the problems of unfavorable industrial production, cumbersome operation process, long reaction time, etc., and achieve the reduction of heating and cooling steps and safe operation Convenience and good product quality
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Embodiment 1
[0033] Add phenylhydrazine (490ml, 4.98mol) dropwise into the mixture of ethyl acetoacetate (636ml, 4.98mol) and acetic acid (28.5ml, 0.498mol), stir, control the rate of addition, keep the reaction temperature at 40-45°C, and complete the dropwise addition Afterwards, the reaction was continued for 20 min, water (2000 ml) was added, solids were precipitated, filtered, and dried to obtain 840 g of crude product Edaravone, with a yield of 96.8%, and a product purity of 98.6% through HPLC analysis.
[0034] mp: 127.1-127.9°C.
Embodiment 2
[0036] Add phenylhydrazine (490ml, 4.98mol) dropwise into the mixture of ethyl acetoacetate (636ml, 4.98mol) and acetic acid (285ml, 4.98mol), stir, control the rate of addition, and keep the reaction temperature at 40-45°C. , continued to react for 20min, added water (2000ml), precipitated solid, filtered, and dried to obtain crude product Edaravone 833g, yield 96.0%, product purity 98.8% through HPLC analysis.
[0037] mp: 127.2-128.1°C.
Embodiment 3
[0039]Phenylhydrazine (490ml, 4.98mol) was added dropwise into a mixture of ethyl acetoacetate (636ml, 4.98mol) and hydrochloric acid (500ml, 5.98mol), stirred, and the rate of addition was controlled to keep the reaction temperature at 70°C. After the addition was complete, continue After reacting for 50 minutes, water (2000ml) was added to precipitate a solid, which was filtered and dried to obtain 810g of crude Edaravone with a yield of 93.3%. The purity of the product was analyzed by HPLC to be 97.2%.
[0040] mp: 127.0-128.0°C.
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