Synthetic Route of 627-31-6, These common heterocyclic compound, 627-31-6, name is 1,3-Diiodopropane(stabilized with Copper chip), 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 3 STR18 3-acetylthiopropyliodide (10) To a solution of 1,3-diiodopropane (10 g, 33.8 mmol) in 10 ml of anhydrous DMF at 0 C. under nitrogen is added, via a cannula over 15 min, a solution of potassium thioacetate (1.3 g, 11.3 mmol) in 5 ml of DMF and the mixture is stirred at 0 C. for 0.5 h, quenched with water (20 ml) and extracted with ether (3*20 ml). The extracts are combined, washed with brine and dried over MgSO4, filtered and concentrated. The residue is purified by flash chromatography (silica gel, EtOAc:hexane/5:95-10:90) to yield iodide 10 (2.5 g, 90%) as a light yellow oil. IR (neat) 2960, 2920, 1689, 1418, 1350, 1210, 1130 cm-1; 1 H NMR (CDCl3) delta 2.00 (2H, m), 2.26 (3H, s), 2.87 (2H, t, J=7 Hz), 3.13 (2H, t, J=6.9 Hz); 13 C NMR (CDCl3) delta 4.35, 29.70, 30.63, 32.97, 195.09.
The synthetic route of 627-31-6 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; Merck Frosst Canada & Co.; US6121253; (2000); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com