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.
452-79-9, 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. 452-79-9, name is 2-Fluoro-1-iodo-4-methylbenzene, A new synthetic method of this compound is introduced below.
Step 7: The product from the previous step was dissolved in dry toluene (8mL) under argon. A portion of this stock solution (ImL) was added to a reaction-vial in a Mettler-Toledo Bohdan block using an atmosphere of argon to exclude air. 2-Fluoro-l-iodo-4-methyl-benzene (0.33mmol; prepared from 2-fluoro-4-methyl-phenylamine according to a general literature procedure [S. E. Tunney and J. K. Stille, J. Org. Chem., 52, 748-53 (1987)]) was added as a toluene solution (ImL) followed by 0.5mL of a freshly prepared toluene stock of solution of tris(dibenzylideneacetone)dipalladium(0) (Pd2dba3) and bis[(2-diphenyl- phosphanyl)phenyl] ether DPEphos (corresponding to 0.3 equivalents palladium and 0.6 equivalents DPEphos). Potassium t¡ãt-butoxide (0.66mmol) was added followed by tetra-n- butyl ammonium fluoride (TBAF; 1.0M in THF; 80 microliter). The mixture was stirred at 1000C overnight under argon. Next morning, the volatiles were removed using a Genevac instrument. The residue was dissolved in methanol (4mL) and loaded onto a VacMaster SCX- column (activated with 10% acetic acid in methanol). The product was eluted with acetonitrile. The volatiles were removed in vacuo. The residue was dissolved in methanol (1.5mL) and 4M HCl in diethyl ether (1.5mL) was added. The mixture was shaken at room temperature over the weekend before the volatiles were removed in vacuo. The residue was dissolved in dimethyl sulfoxide (0.18mL) and filtered. A few drops of 20% acetonitrile in water were added, and the mixture was filtered again. The product was isolated by preparative LC/MS as described, concentrated in vacuo, and the product was dissolved in dimethyl sulfoxide (0.78mL) to give a 1OmM solution. LC/MS-data: Method 14, retention time (UV) 2.152 min; UV-purity 79.5%; ELS-purity 100%; mass observed 337.407.
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; H. LUNDBECK A/S; WO2009/76961; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com