These common heterocyclic compound, 31599-61-8, name is 4-Iodo-1,2-dimethylbenzene, 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. category: iodides-buliding-blocks
Step 1: (3,4-Dimethyl-phenyl)-phenethyl-amine A dried flask was charged with 21 mg (0.11 mmol) CuI and 1.4 g (4.3 mmol) cesium carbonate under argon. 0.40 ml (3.2 mmol) phenethylamine, 0.5 g (2.1 mmol) 4-iodo-0-xylene in solution in 1 ml dried DMF and finally 0.058 ml (0.43 mmol) 2-acetylcyclohexanone were successively added. The mixture was stirred at room temperature for 24 hours. The mixture was diluted with water. The aqueous layer was extracted twice with ethyl acetate. The combined extracts were dried over Na2SO4, filtered and concentrated in vacuo. The crude oil was purified with flash column chromatography on silica eluding with a gradient formed from heptane and ethylacetate to provide 0.10 g (22%) of the title compound as a yellow oil. MS (m/e): 226.2 (MH+).
The synthetic route of 4-Iodo-1,2-dimethylbenzene has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Knust, Henner; Nettekoven, Matthias; Pinard, Emmanuel; Roche, Olivier; Rogers-Evans, Mark; US2009/36422; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com