Synthetic Route of 1746-25-4, A common heterocyclic compound, 1746-25-4, name is 2,4,5-Triiodo-1H-imidazole, molecular formula is C3HI3N2, 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.
To a yellow solution of 2,4, 5-triiodo-1 /-/-imidazole (15.295 g; 34.313 mmol) in anhydrous DMF (200 ml) was added portionwise, at rt, 55-65% sodium hydride moistened with oil (2.058 g; 51.469 mmol). The resulting mixture was further stirred at rt, under nitrogen, for 20 min. The mixture was then heated to 1000C, and a colorless homogeneous solution of 2-(Boc-amino)-ethylbromide (11.534 g; 51.469 mmol) in anhydrous DMF (100 ml) was added dropwise, over 1 h, with an addition funnel. After completion of the addition, the resulting mixture was further heated at 1000C for 1 h. The reaction mixture was cooled to 00C, and water (200 ml) was added slowly. This mixture was extracted with ether (5 x 200 ml). The combined organic layers were washed with brine (100 ml), dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure to give a yellow oil. The crude was purified by FC (heptane / EA = 3 / 2) to give the pure product [2-(2,4,5- triiodo-imidazol-1-yl)-ethyl]-carbamic acid tert-butyl ester as a colorless solid which was further dried under HV (8.540 g; 42%). LC-MS: tR = 0.93 min.; [M+H]+ = 589.89 g/mol.
The synthetic route of 1746-25-4 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; ACTELION PHARMACEUTICALS LTD; WO2008/78291; (2008); A1;,
Imidazole – Wikipedia,
Imidazole | C3H4N2 – PubChem