Reference of 61272-76-2, These common heterocyclic compound, 61272-76-2, name is 4-Fluoro-2-iodoaniline, 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.
N-(4-Fluoro-2-iodophenyl)methanesulfonamide (Ian-09) Methanesulfonyl chloride (1.37 g, 0.94 ml, 12 mmol) was added dropwise at room temperature to a solution of 4-fluoro-2-iodoaniline (Ian-04) (2.38 g, 10 mmol) and 4-(dimethylamino)pyridine (121 mg, 1 mmol) in anhydrous pyridine (25 ml) and then the mixture was refluxed whilst stirring for 12 h. The mixture was cooled to room temperature, diluted with dichloromethane (100 ml) and washed with 5percent hydrochloric acid (3*20 ml) and water (3*20 ml). The organic phase was dried with sodium sulfate and concentrated to small volume under vacuum. Toluene was added repeatedly to the residue, which was concentrated to small volume again under vacuum each time. The crude product (2.91 g) was purified by flash chromatography (100 g, 3.7*20 cm) with cyclohexane/ethyl acetate (4:1). Yield: 2.25 g (71percent), beige-coloured solid Melting point: 90-92° C. 1H-NMR (DMSO-d6): 3.03 (s, 3H); 7.29 (m, 1H); 7.41 (dd, 1H, J=5.5, 8.8 Hz); 7.80 (dd, 1H, J=2.9, 8.2 Hz); 9.33 (s, 1H).
The synthetic route of 61272-76-2 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; GRUNENTHAL GMBH; US2009/215725; (2009); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com