Application 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.
-78 CCooled titanium-dichloride(Cp 2 TiCl 2, 59.8 mg, 0.24 mmol) in ether (2.4 mL)To the solution was added i-propyl magnesium chloride (2.0 M in ether solution, 0.24 mL, 0.48 mmol)1,4-Dioxane (46 [mu] L, 0.54 mmol)And n-tridecafluorohexyl iodide (C 6 F 13 I, 78 muL, 0.36 mmol) were charged, then the temperature was adjusted to -50 C. and stirred for 2 hours.Subsequently, benzaldehyde (20 muL, 0.20 mmol) was added, the temperature was raised, and the mixture was stirred at room temperature for 1 hour.After completion of the reaction, 1 N hydrochloric acid was added to terminate the reaction, followed by extraction with ether three times. The organic layers were combined, dried over sodium sulfate, filtered, and the solvent was distilled off under reduced pressure to obtain a crude product. The obtained crude product was purified by silica gel column chromatography (hexane / ethyl acetate = 20/1 (v / v)) to obtain 2,2,3,3,4,4,5,5,6, 6,7,7,7-tridecafluoro-1-phenyl-1-hydroxyheptane (85.2 mg, yield:> 99%).
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; TOKYO INSTITUTE OF TECHNOLOGY; TOSOH F-TECH INCORPORATED; MIKAMI, KOICHI; FUJIU, MOTOHIRO; (46 pag.)JP5894739; (2016); B2;,
Iodide – Wikipedia,
Iodide – an overview | ScienceDirect Topics – ScienceDirect.com