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. category: iodides-buliding-blocks
EXAMPLE 12 2-Amino-5-chloro-N-cyclohexyl-N-methyl-3-trifluoromethylbenzylamine and its hydrochloride by method B A solution of 9.5 gm of 2-amino-N-cyclohexyl-N-methyl-3-trifluoromethyl-benzylamine and 3 ml of pyridine in 40 ml of tetrahydrofuran was cooled to -10¡ãC, and while stirring at this temperature it was admixed in the course of 20 minutes with a solution of 9.1 gm of iodobenzene dichloride in 80 ml of tetrahydrofuran. After stirring it for 4.5 hours at 0¡ã to -10¡ãC, the mixture was allowed to stand for 18 hours at 20¡ãC. Thereafter, the reaction mixture was diluted with water and extracted with chloroform. The organic phase was washed with aqueous potassium carbonate and water, and after drying it over magnesium sulfate, the solution was evaporated in vacuo, and the oily residue, the free base 2-amino-5-chloro-N-cyclohexyl-N-methyl-3-trifluoromethyl-benzylamine, was taken up in ethyl acetate. The hydrochloride of the base was precipitated from this solution with isopropanolic hydrochloric acid. After recrystallizing the salt three times from ethanol in the presence of charcoal, colorless crystals were obtained which had a melting point of 260¡ã-262¡ãC.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 2401-21-0, its application will become more common.
Reference:
Patent; Boehringer Ingelheim GmbH; US3950393; (1976); A;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com