Extracurricular laboratory: Synthetic route of 2-Chloro-4-fluoro-1-iodobenzene

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 101335-11-9, name is 2-Chloro-4-fluoro-1-iodobenzene, A new synthetic method of this compound is introduced below., name: 2-Chloro-4-fluoro-1-iodobenzene

Step I: 2-Chloro-4-fluoroiodobenzene (9.03g, 35.22mmol, 2.00eq), potassium hydroxide solution (4M, 22.01mL,5.00eq) and bis(triphenylphosphine)palladium dichloride (617.94mg, 880.50umol, 0.05eq) were added to a solution of11 (8.30g, 17.61mmol, 1.00eq) in 100mL dimethyltetrahydrofuran. The reaction solution was stirred at 70C undernitrogen atmosphere for 12 hours, then filtered through celite, and the filtrate was washed twice with 100mL brine. Theorganic phase was dried over anhydrous sodium sulfate, filtered and concentrated to give a crude product, which waspurified by silica gel column chromatography (PE:EA=40:1-10:1) to give the product 13 as a yellow solid (4.50g, 5.57mmol,yield 31.65%, purity 58.7%). MS [ESI, M+1]: 474.3.

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

Reference:
Patent; Luoxin Biotechnology (Shanghai) Co., Ltd.; Shandong Luoxin Pharmaceutical Group Stock Co., Ltd.; LU, Jianyu; DING, Charles Z.; HU, Lihong; HE, Huijun; CHEN, Shuhui; DONG, Jiaqiang; WANG, Tie-lin; (124 pag.)EP3434668; (2019); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com