Reference of 118-69-4, In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 118-69-4 as follows.
Example 1Preparation of DCDNTTo a 1 L 3-neck round bottom flask equipped with external ice cooling, mechanical stirrer, addition funnel, N2 inlet, and thermometer was added 174 g (2.76 mol) fuming nitric acid (d=1.54), followed by 350 g sulfuric acid and 659 g 30% oleum (2.0 molar equiv SO3) maintaining a temperature between 5 and 20 C. Subsequently, 199 g (1.23 mol) 1,3-dichlorotoluene (99% purity, Aldrich Chemical Company, Milwaukee, Wis., USA) was added over a time period of 3 h while maintaining a temperature between 0 C.-10 C. The ice bath was removed, and the reaction mixture was allowed to warm up to room temperature. It was then heated to 100 C. for about 2 h. To analyze the reaction mixture, a small sample of crude product was taken from the reaction vessel and poured into ice water. The crude product was extracted with methylene chloride. Analysis by GC indicated a reaction selectivity to 3,5-dinitro-2,6-dichlorotoluene of >97%. Subsequently, the reaction mixture was allowed to cool to room temperature over 2 h and then cooled to 5 C. over 30 min, after which it was filtered through a glass fritted funnel and washed with a little sulfuric acid followed by 200 mL H20. The wet cake contained about 20% water. After drying, 291 g of >99.5% pure DCDNT product (by 1H-NMR) was isolated (93.5% net yield).
According to the analysis of related databases, 118-69-4, the application of this compound in the production field has become more and more popular.
Reference:
Patent; E. I. DU PONT DE NEMOURS AND COMPANY; US2010/160685; (2010); A1;,
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