Reference of 34270-90-1, These common heterocyclic compound, 34270-90-1, name is 1-Iodo-2-(2-iodoethoxy)ethane, 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.
Step 1 :NaH (60% in oil, 975 mg, 24.38 mmol) is washed with pentane (3x) and then suspended in dry THF (10 mL). A solution of 4,4-dimethyl cyclohexanone (1.02 g, 8.12 mmol, Combi-Blocks) in THF (5 mL) is added, followed by bis-2-iodoethyl ether (1.25 mL, 8.80 mmol). The reaction mixture is heated to 65C. When an exothermic reaction occurs, external heating is stopped and the reaction mixture is stirred for 1.5 h. The reaction mixture is heated at reflux for 30 min, and then is poured into water and extracted with ether. The aqueous phase is acidified to pH 6 with 1 M HCI and extracted with ether (2x). The filtrate is dried over anhydrous Na2S04, concentrated under reduced pressure and purified by Combiflash (90:10Hex EtOAc) to afford 6a1.
The synthetic route of 34270-90-1 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; BOEHRINGER INGELHEIM INTERNATIONAL GMBH; BROCHU, Christian; GRAND-MAITRE, Chantal; FADER, Lee; KUHN, Cyrille; BERTRAND-LAPERLE, Megan; PESANT, Marc; WO2013/26163; (2013); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com