Reference of 31599-61-8, A common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, molecular formula is C8H9I, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.
14 Typical procedure for the preparation of 4,5-disubstituted-1,2,3-(NH)-triazoles (synthesis of 3a): A round-bottom sidearm flask (10 mL) containing PdCl2(PPh3)2 (0.015 mmol) was subjected to the Schlenk-line procedures of evacuation and purging of CO for three cycles. Iodobenzene and 4 equiv Et3N (1.2 mmol) were successively added, and the mixture was stirred at room temperature for 10 min, then 1-hexyne (0.45 mmol) was added, continuously stirred at room temperature for 14 h. Then NaN3 (35.1 mg, 0.54 mmol) and 1 mL DMSO were added to the mixture and the reaction continued at 45 C for 36 h. Following, to the reaction mixture was added water (2 mL), 20% HCl solution (1 mL) and extracted with ether (3 * 10 mL). The combined organic phases were washed with brine (2 * 5 mL), dried over anhydrous MgSO4 and concentrated in vacuo. The residue was subjected to flash column chromatography with hexanes/EtOAc (5/1) as eluent to obtain the desired 3a (56.33 mg, 82% yield). All products gave satisfactory spectroscopic and analytical data.
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:
Article; Li, Na; Wang, Dong; Li, Jihui; Shi, Weilin; Li, Chao; Chen, Baohua; Tetrahedron Letters; vol. 52; 9; (2011); p. 980 – 982;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com