Category: 41252-98-6

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 41252-98-6 as follows. Safety of 1-Iodo-2-methyl-3-nitrobenzene

Step 2 3-(2-Iodo-6-nitro-phenyl)-2-oxo-propionic acid Sodium ethoxide solution (35 ml, 44 mmol) in an ice-water bath was added dropwise with a solution of 1-iodo-2-methyl-3-nitro-benzene 74b in ethanol (35 ml, 40 mmol) under an argon atmosphere. Upon completion of the addition, the reaction mixture was stirred until lots of brown precipitates were formed, and added with diethyl oxalate (6 ml, 44 mmol) in one portion. The reaction mixture was refluxed at 100 C. in an oil bath for 0.5 hour, added with water (70 ml) and refluxed for another 1 hour. The reaction mixture was concentrated under reduced pressure to evaporate ethanol, washed with ethyl acetate (50 ml) under base condition, adjusted to pH 3 with hydrochloric acid (1M), and extracted with ethyl acetate (30 ml*3). The combined organic extracts were washed with saturated brine (30 ml), dried over anhydrous sodium sulfate, filtered and concentrated under reduced pressure to obtain the title compound 3-(2-iodo-6-nitro-phenyl)-2-oxo-propionic acid 74c (2.94 g) as a brown oil to be used directly in the next step.

According to the analysis of related databases, 41252-98-6, the application of this compound in the production field has become more and more popular.

Reference:
Patent; ChoTang, Peng Cho; Su, Yidong; Li, Yali; Zhang, Lei; Zhao, Fuqiang; Yang, Jialiang; Zhou, Ying; Bie, Pingyan; Qian, Guangtao; Ju, Minggang; US2010/75952; (2010); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 41252-98-6, name is 1-Iodo-2-methyl-3-nitrobenzene, This compound has unique chemical properties. The synthetic route is as follows., HPLC of Formula: C7H6INO2

4.1.11. 2,20-Dimethyl-3,30-dinitro-1,10-biphenyl (27)4.1.11.1. Activation of copper powder:.34 Copper powder (2.00 g)was stirred with 2% iodine (w/w wrt copper) in acetone (100 mL)for 10 min. The powder was filtered and stirred to form a slurrywith 1:1 solution of concentrated hydrochloric acid in acetone(200 mL). The copper iodide dissolved, and the copper powderremaining was removed by filtration and washed with acetone(200 mL). The activated copper was dried in a vacuum desiccatorand used immediately.2-Methyl-3-nitro-iodobenzene (26) (1.00 g, 3.80 mmol) andactivated copper (1.21 g, 19.0 mmol) were added to dry N,Ndimethylformamide(8 mL), and the mixture was heated to 190 Cfor 24 h. The mixture was diluted with dichloromethane (100 mL),washed with 4% aqueous ammonia (5100 mL), water (450 mL),and brine (350 mL), dried (Na2SO4), and the solvents removedunder reduced pressure to yield a dark crude oil. Column chromatographyof the residue using ethyl acetate/petroleum ether(1:10) gave the product as a yellow solid (0.27 g, 53%); mp120e121 C; nmax (film)/cm1 3086, 1604, 1524, 1458, 1350, 1279,1219, 1106, 995, 859, 807, 736, 718, 674; 1H NMR (400 MHz, CDCl3):d 2.13 (6H, s, 2 CH3), 7.29 (2H, dd, J7.6, 1.4 Hz, 2 CH arom., biphenyl-5,50), 7.36 (2H, ddd, J8.0, 7.6, 0.5 Hz, 2 CH arom., biphenyl-6,60), 7.83 (2H, dd, J8.0, 1.4 Hz, 2 CH arom., biphenyl-4,40); 13CNMR (100 MHz, CDCl3): d 15.4 (2 CH3, 2 ArCH3), 123.1 (2 CHarom., biphenyl-4,40),125.7 (2 CH arom., biphenyl-5,50),129.8 (2 Cquat., arom., biphenyl-2,20), 132.6 (2 CH arom., biphenyl-6,60), 141.3(2 C quat., arom., biphenyl-1,10), 149.9 (2 C quat., arom., biphenyl-3,30); m/z (EI) 272.0793; C14H12N2O4 (M) requires 272.0797.

According to the analysis of related databases, 41252-98-6, the application of this compound in the production field has become more and more popular.

Reference:
Article; Farah, Mohamed M.; Page, Philip C. Bulman; Buckley, Benjamin R.; Blacker, A. John; Elsegood, Mark R.J.; Tetrahedron; vol. 69; 2; (2013); p. 758 – 769;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com

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