Synthetic Route of 3032-81-3, A common heterocyclic compound, 3032-81-3, name is 1,3-Dichloro-5-iodobenzene, molecular formula is C6H3Cl2I, 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.
Example 87BN-[(2Z)-3-(3,5-dichlorophenyl)-5-methyl-1,3-thiazol-2(3H)-ylidene]-2,2-dimethylpropanamide; In a 4 mL vial charged with a stir bar, 2,2-dimethyl-N-(5-methyl-1,3-thiazol-2-yl)propanamide (71 mg, 0.35 mmol) was added, followed by copper(I) trifluoromethanesulfonate benzene complex (35 mg, 0.07 mmol), 5-chloro-1,10-phenanthroline (30 mg, 0.14 mmol) and cesium carbonate (126 mg, 0.39 mmol). A loose cap with septum was placed on the vial and the vial was placed under vacuum in a vacuum oven for 30 minutes. The solid mixture was purged with nitrogen gas a couple of times. Then 1,3-dichloro-5-iodobenzene (115 mg, 0.42 mmol) dissolved in 1-methyl-2-pyrrolidinone (1.0 mL) was added to the solid mixture. The vial was capped and placed on a heater/stirrer and heated to 120° C. overnight. Then a 1 mL solution of concentrated ammonium hydroxide/water (1:2) was added. The reaction was filtered and concentrated to dryness. The residue was purified by reverse phase HPLC (C8, gradient 10-100percent acetonitrile/water/0.1percent trifluoroacetic acid).1H NMR (500 MHz, DMSO-d6/D2O) delta ppm 1.08-1.12 (m, 9H) 2.25-2.31 (m, 3H) 7.41-7.47 (m, 1H) 7.68 (t, 1H) 7.81-7.85 (m, 2H); MS (ESI) m/z 343 (M+H)+.
The synthetic route of 3032-81-3 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ABBOTT LABORATORIES; US2009/163470; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com