Related Products of 14452-30-3, 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 14452-30-3 as follows.
General procedure: Single-pass manner (conditions A and B): A solution of iodoarene (1mmol), alkene (2mmol), and Bu3N (condition A, 1.5mmol; condition B, 3mmol) in DMA (condition A, 10mL; condition B, 4mL) was prepared in a vial and flowed into cartridge A packed with 7% Pd/WA30 at the flow rate of 0.15mLmin-1 along with the MW irradiation (10W) under the 1MPa back-pressure in a single-pass manner. After the entire solution in the vial had passed through the catalyst cartridge, additional DMA (15mL) was passed through the path to wash out the remaining reagents (total operation time: ca. 140 min). To the collected mixture were added EtOAc (20mL) and H2O (10mL), and the layers were separated. The aqueous layer was extracted with EtOAc (20mL). The combined organic layers were washed with H2O (20mL×4) and brine (20mL), dried over Na2SO4, and concentrated in vacuo. To the residue was added CDCl3 (ca. 1.5mL) and 1,4-dioxane (8.53muL, 100mumol) as an internal standard, and the yield was determined by 1H NMR. The 1H NMR sample was diluted with EtOAc (15mL), washed three times with sat. aq. CuSO4 (5mL) and H2O (10mL), dried over Na2SO4, concentrated in vacuo. The residue was purified by silica gel column chromatography using hexane/EtOAc (10: 1) as the eluent to give the corresponding substituted alkenes as the Mizoroki-Heck reaction product. (0023) Circulation manner (condition C): When the TLC analysis revealed that the aryl iodide still remained unreacted after a single-pass of the reaction solution through the catalyst cartridge, both the starting and ending parts of the flow path were dipped into the reaction solution in a reservoir for circulation. After 7.5h of circulation at the flow rate of 0.15mLmin-1, the flow path was washed with DMA (15mL). The recovered mixture was treated according to a procedure similar to that described for the single-pass setup.
According to the analysis of related databases, 14452-30-3, the application of this compound in the production field has become more and more popular.
Reference:
Article; Ichikawa, Tomohiro; Mizuno, Masahiro; Ueda, Shun; Ohneda, Noriyuki; Odajima, Hiromichi; Sawama, Yoshinari; Monguchi, Yasunari; Sajiki, Hironao; Tetrahedron; vol. 74; 15; (2018); p. 1810 – 1816;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com