3,5-Dinitrosalicylic acid synthesis
- Product Name:3,5-Dinitrosalicylic acid
- CAS Number:609-99-4
- Molecular formula:C7H4N2O7
- Molecular Weight:228.12
69-72-7
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609-99-4
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Yield:609-99-4 84%
Reaction Conditions:
in conc. nitric acid;sulfuric acid;water
Steps:
P.4 Preparation of 3,5-dinitrosalicylic acid (DNSA)
Production Example 4 Preparation of 3,5-dinitrosalicylic acid (DNSA) In a 3-liter reactor, 138 g salicylic acid was immersed in 588 g of 98% conc. sulfuric acid with stirring slowly to avoid agglomeration. The reactor was placed in a ice-water bath and 190 g of 98% conc. nitric acid was added drops into the above solution over 1.5 hours by using addition funnel with controlling addition rate under maintaining the reaction temperature at 20~40° C. while stirring. While maintaining in ice-water bath, 1.5 L iced water was quickly added into the resultant solution to quench the nitration. During the addition, it should be careful due to the exothermic reaction. After continuously stirring for 15 minutes, the solid was filtered and washed by 500 mL pure water to obtain solid 3,5-dinitrosalicylic acid (NNSA) in yellow color. Yield: 84% (m.p.: 167.7° C., DSC).
References:
HWANG, Kuen Yuan;Tu, An Pang;Wu, Sheng Yen;Chen, Gai Chi;Huang, Ching Jui;Wang, Jen Fu US2011/172324, 2011, A1
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