Reference of 29289-13-2, 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. 29289-13-2, name is 2-Iodo-4-methylaniline belongs to iodides-buliding-blocks compound, it is a common compound, a new synthetic route is introduced below.
Step 2: Preparation of 1-bromo-2-iodo-4-methylbenzene To a mixture of 2-iodo-4-methylaniline (50 g, 214.55 mmol) in HOAc (250 mL), H2SO4 (10 mL), and H2O (40 mL) was added a solution of NaNO2 (14.5 g) in H2O (80 mL) at 0 C. The solution was stirred for 1.5 h. This was defined as mixture A. In another round bottom flask, a mixture of NaBr (107 g), CuSO4 (32.2 g), Cu (38.9 g), H2SO4 (39 mL), and H2O (25 mL) was refluxed for 1.5 h. To this mixture was added mixture A, and the solution was then refluxed for 3 h. The solution was treated with water and extracted with EA (500 mL*3). The combined organic layers were washed with brine, dried over Na2SO4, and then concentrated in vacuo. Purification by column chromatography over silica gel eluted with PE afforded the product as colorless oil (43 g, yield 68%). 1H NMR (300 MHz, CDCl3): delta 7.69 (m, 1H), 7.47 (d, J=8.1 Hz, 1H), 7.00 (m, 1H), 2.26 (s, 3H) ppm.
The synthetic route of 2-Iodo-4-methylaniline has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Anacor Pharmaceuticals, Inc.; Eli Lilly and Company; Akama, Tsutomu; Balko, Terry William; Defauw, Jean Marie; Plattner, Jacob J.; White, William Hunter; Winkle, Joseph Raymond; Zhang, Yong-Kang; Zhou, Yasheen; US2013/131016; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com