Reference of 41252-98-6, In the next few decades, the world population will flourish. As the population grows rapidly and people all over the world use more and more resources, all industries must consider their environmental impact. 41252-98-6, name is 1-Iodo-2-methyl-3-nitrobenzene belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
1) Under argon protection,Iodoacetic acidEthyl ester,Magnesium ethoxide,The catalyst was mixed with anhydrous tetrahydrofuran to control the reaction temperature to rise to 112 C.The pressure rises to 4.5 atmospheres,Mixing a mixture of 6-iodo-2-nitrotoluene in anhydrous isopropanol,The control dropping time is 50 min, and after the end of the dropwise addition, the control temperature is raised to 140 C.The pressure was raised to 8 atmospheres, and the reaction was continued for 3 hours and then cooled to room temperature.Add 12% by mass aqueous sodium hydroxide solution, and control the temperature not to exceed 90 C.After the dropwise addition of the aqueous sodium hydroxide solution, the temperature was controlled to rise to 132 C.The pressure is 2.6 atmospheres and the reaction ends at 1.5 hours.The preparation method of the catalyst is as follows: the nano molecular sieve is immersed in a mass fraction of 5% sodium hydroxide solution for 2.5 days, filtered, washed with water and activated at 700 C.Ethyl iodine, 6-iodo-2-nitrotoluene,The molar ratio of magnesium ethoxide is 1:0.58:1.1; ethyl iodide,The ratio of the catalyst to anhydrous tetrahydrofuran is 1 g: 0.2 g: 4 mL;The ratio of 6-iodo-2-nitrotoluene to anhydrous isopropanol is 1 g: 3.5 mL;The molar ratio of 6-iodo-2-nitrotoluene to sodium hydroxide in aqueous sodium hydroxide solution was 1:2.3.2) After cooling, the precipitate is removed by filtration, and the obtained filtrate is adjusted to pH 1 with 20% hydrochloric acid, extracted with chloroform, and the layers are separated. The organic layer is washed with water and dried over anhydrous sodium sulfate Get the product. The molar yield was 99.5% and the GC purity was 99.2%.
The synthetic route of 1-Iodo-2-methyl-3-nitrobenzene has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Shenzhen The Second People Hospital; Tan Hui; Li Weiping; Huang Guodong; (7 pag.)CN109810001; (2019); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com