In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 134450-56-9 as follows. 134450-56-9
General procedure: The synthesis was largely adopted from literature. (reference 4) To a solution ofcarbazole (2.0 g, 12.0 mmol, 1 equiv.) in dry THE (40 mL) at room temperature wasportionwise added sodium hydride (60% in mineral oil, 0.96 g, 24.0 mmol, 2 equiv.). The suspension was stirred under nitrogen protection for 15 minutes. 4,5- difluorophthalonitrile (1.2 g, 0.72 mmol, 0.6 equiv.) was added. The colour of the suspension changed from milky to red immediately and it was allowed to stir for further3 h. Green emission (upon excitation with 365 nm UV light) slowly developed during the course of the reaction. The suspension was then slowly added to ice water and then the mixture was extracted with DCM (3 x 25 mL). The combined organic layers were dried with anhydrous sodium sulfate and concentrated under reduced pressure. The crude mixture was purified by flash column chromatography using DCM : Hexanes= 3 : 2 as eluent to afford the title compound. Green solid. Yield: 74%. R: 0.39 (EtOAc Hexanes = 1:4 on silica). Mp: 332-333C. 1H NMR (300 MHz, CDCI3) oe (ppm): 8.33 (s, 2 H), 7.82-7.79 (m, 4 H), 7.16-7.06 (m, 12 H). 13C NMR (76 MHz, CDCI3) oe (ppm):138.4, 138.2, 135.5, 126.2, 124.3, 121.7, 120.4, 114.7, 114.5, 109.0.
According to the analysis of related databases, 134450-56-9, the application of this compound in the production field has become more and more popular.
Reference:
Patent; UNIVERSITY COURT OF THE UNIVERSITY OF ST ANDREWS; ZYSMAN-COLMAN, Eli; WONG, Michael Yin; (74 pag.)WO2016/174377; (2016); A1;,
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