Synthesis method of 3,5-dimethyl-4-nitropyridine-N-oxide
A technology of lutidine and nitropyridine, applied in the field of synthesis of 3,5-dimethyl-4-nitropyridine-N-oxide, which can solve serious problems, equipment corrosion, bad operating environment, etc. , to achieve the effect of short reaction time, high product yield and friendly operation environment
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Embodiment 1
[0022] Dissolve 12.3g of 3,5-lutidine-N-oxide in 90g of concentrated sulfuric acid, add dropwise a sulfuric acid solution of potassium nitrate (potassium nitrate 14.15g, concentrated sulfuric acid 100g ). After the dropwise addition was completed, the reaction was carried out at a temperature of 60° C. to 65° C. for 2 hours. HPLC monitoring until complete reaction of starting material. Cool down to room temperature, add water and stir, adjust pH to 8-8.5 with ammonia water, filter and dry to obtain 14.4 g of light yellow 3,5-dimethyl-4-nitropyridine-N-oxide, HPLC purity 99%, yield The rate is 85.7%.
Embodiment 2
[0024] Dissolve 12.3g of 3,5-lutidine-N-oxide in 188g of concentrated sulfuric acid, add dropwise a sulfuric acid solution of potassium nitrate (40.44g of potassium nitrate, 600g of concentrated sulfuric acid) at a temperature of 20°C to 30°C ). After the dropwise addition was completed, the reaction was carried out at a temperature of 110° C. to 120° C. for 0.5 hours. HPLC monitoring until complete reaction of starting material. Cool down to room temperature, add water and stir, adjust the pH to 8-8.5 with ammonia water, filter, and dry to obtain 14.5 g of light yellow 3,5-dimethyl-4-nitropyridine-N-oxide, HPLC purity 99%. The yield is 86.3%.
Embodiment 3
[0026] Dissolve 12.3g of 3,5-lutidine-N-oxide in 65g of concentrated sulfuric acid, and dropwise add sulfuric acid solution of potassium nitrate (potassium nitrate 10.11g, concentrated sulfuric acid 60g) at a temperature of 10°C to 15°C ). After the dropwise addition is completed, the reaction is carried out at a temperature of 85° C. to 90° C. for 1 hour. HPLC monitoring until complete reaction of starting material. Cool down to room temperature, add water and stir, adjust pH to 8-8.5 with ammonia water, filter and dry to obtain 14.3 g of light yellow 3,5-dimethyl-4-nitropyridine-N-oxide, HPLC purity 99%, yield rate of 85%.
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