Method for synthesizing bendamustine hydrochloride intermediate
A technology of bendamustine hydrochloride and a synthesis method, which is applied in the field of chemical synthesis, can solve the problems of low selectivity of reduction, a large amount of sodium sulfide waste water, environmental pollution and the like, and achieves the advantages of shortening production cycle, short route and reducing cost. Effect
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[0018] Take 51.6g of 2-chloro-5-nitroaniline into a three-neck flask, add 500ml of toluene, add 36g of glutaric anhydride at room temperature, heat to 80°C for 3 hours, cool to room temperature, filter, and filter cake at 70°C After drying, 145 g of a yellow solid intermediate was obtained, with a yield of 95%.
[0019] Add intermediate 1 obtained above into 150ml of 40% methylamine aqueous solution, heat to 50°C for 3 hours, cool to room temperature, adjust pH to 4-5 with 2N hydrochloric acid, precipitate a yellow solid, stir for 1 hour, filter, filter The cake was rinsed with toluene and dried at 70°C to obtain 40.5 g of yellow solid intermediate 2 with a yield of 91.7%.
[0020] Put the intermediate 2 prepared above into a three-necked flask, add 365ml of absolute ethanol, add 12ml of 98% concentrated sulfuric acid dropwise under stirring, heat to 80°C and reflux for 3h after the dropwise addition, cool to 45-50°C, pour the reaction solution into In saturated aqueous potas...
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