Application of 162356-38-9, These common heterocyclic compound, 162356-38-9, name is 2-(2-Bromophenyl)-1H-imidazole, 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.
General procedure: First, 100 mmol 2-phenylimidazole derivative introduced 400 ml of triethylamine. And continuously added with stirring 200 ml alkynyl, 6 mmol triphenylphosphine, 6 mmol of copper iodide (I) and 3 mmol of palladium acetate (II). The reaction mixture was then stirred for 20 hours at 80 . After cooling, the reaction mixture was diluted with 400 ml of methylene chloride, to separate a solid via filtration through a bed of salt C The filtrate was evaporated to dryness. The residue was dissolved in 300 ml of methylene chloride, 100 ml of concentrated aqueous ammonia with individual cleaning solution three times, and then washed three times with 100 ml of water, and dried over magnesium sulfate. After the solvent was removed in vacuo, the crude product was adsorbed onto silica gel (5 grams per gram of crude product silicone), and loaded into a silica gel column. First with dichloromethane to remove byproducts, but will be converted to THF solvent to elute the product. With spherical fractionating tube distillation or sublimation, resulting in the manipulation of the vacuum pump oil / solids release low-boiling components.
The synthetic route of 162356-38-9 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; MERCK PATENT GMBH; STOESSEL, PHILIPP; HEIL, HOLGER; JOOSTEN, DOMINIK; PFLUMM, CHRISTOF; GERHARD, ANJA; BREUNING, ESTHER; (214 pag.)TWI520958; (2016); B;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem