Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 1835-65-0, name is 3,4,5,6-Tetrafluorophthalonitrile, A new synthetic method of this compound is introduced below., HPLC of Formula: C8F4N2
Example 1; Synthesis of hexadecafluorovanadylphthalocyanine; Into a separable flask of glass provided with a stirrer, a thermometer, a water separation tube, and a cooling tube and having an inner volume of 300 ml, a nitrogen gas was introduced at a rate of 500 ml/min for 10 minutes to replace the interior of the reaction vessel with the nitrogen gas. Then, the reaction vessel was charged with 30 gr (0.15 mol) of tetrafluorophthalonitrile, 58.6 gr (0.45 mol) of n-octanol, and 6.9 gr (0.0438 mol) of vanadium trichloride (produced by Sinko Kagaku K.K.). Again, a nitrogen gas was introduced at a rate of 500 ml/min for 10 minutes into the reaction vessel to replace the interior thereof with the nitrogen gas. When the oxygen concentration in the reaction vessel was determined with an oxygen concentration meter, it was found to be 1.8 vol percent. Under the condition of continued stirring, the reaction mixture in the reaction vessel was exposed to a current of nitrogen gas at a flow rate of 30 ml/min and heated. The linear speed of the gas at the inlet part (the connecting part between the reaction vessel and the cooling tube) was 0.6 cm/sec and the oxygen concentration in the reaction vessel was measured with an oxygen concentration meter to be found to be 1.8 vol percent. The temperature was elevated to 150¡ã C. over two hours, then the reaction was further continued for three hours, and the reaction vessel was left cooling to normal room temperature. In the meanwhile, the flow of the nitrogen gas was continued. The conversion of tetrafluorophthalonitrile was determined by liquid chromatography, to find to be 99.2percent. The slurry resulting from the cyclization was filtered to separate a solid component. The solid component was washed with 300 gr of benzonitrile, then washed with 100 gr of methanol, and dried under a reduced pressure at 150¡ã C. for 12 hours. The weight of the target product, hexadecafluorovanadyphthalocyanine, as calculated from the weight after drying, was 28.1 gr (yield: 86.4 mol percent).; Comparative Example 4; When the reaction was performed by following the procedure of Example 1 while omitting the replacement with a nitrogen gas prior to the reaction and the introduction of a nitrogen gas during the course of the reaction, and supplying air at a flow rate of 30 ml/min to the reaction vessel, the weight of hexadecafluorovanadyl phthalocyanine was found to be 12.5 gr (yield: 38.5 mol percent). When the oxygen concentration in the reaction vessel was determined at this time with an oxygen concentration meter, it was found to be 20.3 vol percent.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; Hirota, Kouichi; Hashimoto, Yukihide; Masuda, Kiyoshi; Kitao, Masunori; US2005/203293; (2005); A1;,
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