Some common heterocyclic compound, 17024-12-3, name is 9-Iodophenanthrene, molecular formula is C14H9I, 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. HPLC of Formula: C14H9I
Mixed under argon flow were 100 g of N,N’-diacetyl-4,4′-benzidine (manufactured by Tokyo Kasei Kogyo Co., Ltd.), 337 g of 9-iodophenanthrene, 204 g of anhydrous potassium carbonate (manufactured by Tokyo Kasei Kogyo Co., Ltd.), 4.7 g of copper powder (manufactured by Hiroshima Wako Co., Ltd.) and 750 ml of decalin, and they were reacted at 190C for 3 days. After cooling, 2 liter of toluene was added thereto to filter an insoluble matter. The matter filtered was dissolved in 4.5 liter of chloroform to filter off an insoluble matter, and then the filtrate was treated with activated carbon and concentrated under reduced pressure. Acetone 3 litter was added when the solution became slurry in the middle of concentration, and crystal deposited was filtered and dried. This was suspended in a mixture of 2 liter of ethylene glycol and 20 ml of water, and 110 g of a 85 % potassium hydroxide aqueous solution was added thereto, followed by carrying out reaction at 120C for 12 hours. After left cooling down to a room temperature, the reaction liquid was injected to 4 liter of water and treated with activated carbon, and then it was concentrated under reduced pressure. Acetone was added when the solution became slurry, and crystal deposited was filtered and dried to obtain 116 g of N,N’-bis(phenantho-9-yl)-4,4′-benzidine (A3).
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 17024-12-3, its application will become more common.
Reference:
Patent; IDEMITSU KOSAN CO., LTD.; EP1559706; (2005); A1;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com