5832-44-0

Deliquescent cryst

The general procedure for synthesizing 3-nitro-4-methylpyridine from 4-methylpyridine is as follows:1) In step 1) of Example 1, prepare a reaction solution by adding 60 g of nitrogen pentoxide solid to 300 g of liquid sulfur dioxide at -30° C. and stirring sufficiently until completely dissolved.2) Dissolve 30 g of 4-methylpyridine in 120 g of liquid sulfur dioxide and maintain the temperature at -30° C.3 ) Slowly drop the reaction solution into 300 g of ice water for 5 minutes. ) Slowly add the nitrogen pentoxide-sulfur dioxide solution prepared in step 1) dropwise to the 4-methylpyridine solution, and react for 5 min. 4) Slowly pour the reaction solution into 300 g of ice water, and hydrolyze thoroughly. 5) Adjust the pH of the hydrolyzed solution to 8-9 using sodium carbonate. 6) Add 290 g of toluene for two extractions, and combine the extracts. 7) Remove the solvent by vacuum distillation to obtain 39 g of 3- Nitro-4-methylpyridine. The purity of the product was 99.0% by gas chromatography.

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[3] Acta Chemica Scandinavica, 1994, vol. 48, # 2, p. 181 - 182
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[5] Acta Chemica Scandinavica, 1996, vol. 50, # 6, p. 556 - 557