Synthetic Route of 2401-21-0,Some common heterocyclic compound, 2401-21-0, name is 1,2-Dichloro-3-iodobenzene, molecular formula is C6H3Cl2I, 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.
PREPARATION 5 A mixture of p-aminopropiophenone (5 g), pyridine (2.7 g), and iodobenzene dichloride (7.5 g) in tetrahydrofuran (150 ml) was stirred for 3 hours at 0¡ã to 5¡ã C. The insoluble materials were filtered, and the filtrate was concentrated under reduced pressure. The residue was dissolved in chloroform, washed with an aqueous solution of sodium hydrogen sulfite, dried over magnesium sulfate, and concentrated to give an oil (8.8 g). The oil was subjected to column chromatography on silica gel eluding with chloroform. The fractions containing the desired compound were combined and concentrated under reduced pressure. The residual oil was triturated with a mixture of hexane and ethyl acetate to give pale yellow crystals of 4′-amino-3′-chloropropiophenone (1.1 g). mp: 79¡ã to 80¡ã C. IR (Nujol): 3500, 3380, 1670, 1620, 1595 cm-1. NMR (CDCl3, delta): 1.20 (3H, t, J=7 Hz), 2.88 (2H, q, J=7 Hz), 4.50 (2H, broad s), 6.72 (1H, d, J=8 Hz), 7.68 (1H, dd, J=8 Hz, 2 Hz), 7.88 (1H, d, J=2 Hz).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,2-Dichloro-3-iodobenzene, its application will become more common.
Reference:
Patent; Fujisawa Pharmaceutical Co., Ltd.; US4866091; (1989); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com