Electric Literature of 355-43-1,Some common heterocyclic compound, 355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, molecular formula is C6F13I, 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.
1.Tetramethyl hydrazine (1.0 mmol) was placed in a 25 mL round bottom flask at room temperature.2 mL of acetonitrile (water content 0.1%) solvent was injected, and then perfluoroiodohexane (1.1 eq) was added.The reaction was carried out under 36 W CFL light, and TLC was monitored until the reaction was complete (about 10 h).The obtained reaction product was poured into 100 mL of water, extracted three times with dichloromethane, and the organic phase was dried, and the organic solvent was evaporated under reduced pressure to give a crude product; 2.The crude product was subjected to silica gel column chromatography (silica gel needs to be pretreated with Et3N/PE=1:9 overnight), and eluted with an eluent (petroleum ether: ethyl acetate = 1:1 (V:V)). Eluent, distillation under reduced pressure,Obtained a white solid,It is the product N-[bis(dimethylamino)methylidene]-2,2,3,3,4,4,5,5,6,6,6-undecafluorohexanamide,The yield is 79%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, its application will become more common.
Reference:
Patent; Liaoning University; Liang Fushun; Wang Rui; Su Zhongmin; (13 pag.)CN109369467; (2019); A;,
Iodide – Wikipedia,
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