A kind of method of secondary nitration synthesis 5-nitrobenzimidazolone
A technology of nitrobenzimidazolone and benzimidazolone, which is applied in the field of synthesizing 5-nitrobenzimidazolone, can solve the problems of large product impurity peaks, large environmental pollution, and low safety factor, and achieve stable reaction, The effect of improving product purity and reducing pollution
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Embodiment 1
[0028] A method for secondary nitration to synthesize 5-nitrobenzimidazolone. The steps are: add 60g of benzimidazolone dry product and 347g of nitric acid mother liquor (9% nitric acid mass concentration) to a 1L reactor, and control the temperature at 45 Between -70°C, keep warm for 1 hour. After the material in the reaction kettle turns green, transfer the material liquid to 200g of dilute nitric acid prepared in advance through the metering pump (the mass concentration of nitric acid is 30.58%), and the temperature is controlled at 60-70°C In between, heat preservation for 1 hour, the heat preservation reaction is completed, and the temperature is lowered to 50° C. for hot suction filtration. The filtrate, namely the nitric acid mother liquor, is applied mechanically to the next batch of nitration reactions. After testing, the molar yield was 99.5%, and the purity was 99.33%.
Embodiment 2
[0030] A method for secondary nitration to synthesize 5-nitrobenzimidazolone, the steps are: add 60g of benzimidazolone dry product and 347g of nitric acid mother liquor (9% nitric acid mass concentration) to a 1L reactor, and control the temperature at 25 Between -45°C, keep warm for 1 hour. After the material in the reaction kettle turns green, transfer the material liquid into 200g of dilute nitric acid prepared in advance through the metering pump (the mass concentration of nitric acid is 30.58%), and the temperature is controlled at 60-70°C In between, heat preservation for 1 hour, the heat preservation reaction is completed, and the temperature is lowered to 50° C. for hot suction filtration. The filtrate, namely the nitric acid mother liquor, is applied mechanically to the next batch of nitration reactions. After testing, the molar yield was 99.1%, and the purity was 98.62%.
Embodiment 3
[0032] A method for secondary nitration to synthesize 5-nitrobenzimidazolone. The steps are: add 60g of benzimidazolone dry product and 347g of nitric acid mother liquor (9% nitric acid mass concentration) to a 1L reactor, and control the temperature at 45 Between -70°C, keep warm for 1 hour. After the material in the reaction kettle turns green, transfer the material liquid to 200g of dilute nitric acid prepared in advance through the metering pump (the mass concentration of nitric acid is 25%), and the temperature is controlled at 60-70°C In between, heat preservation for 1 hour, the heat preservation reaction is completed, and the temperature is lowered to 50° C. for hot suction filtration. The filtrate, namely the nitric acid mother liquor, is applied mechanically to the next batch of nitration reactions. After testing, the molar yield was 98.45%, and the purity was 97.89%.
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