355-43-1, name is 1,1,1,2,2,3,3,4,4,5,5,6,6-Tridecafluoro-6-iodohexane, belongs to iodides-buliding-blocks compound, is considered to be a conventional heterocyclic compound, which is widely used in drug synthesis. The chemical synthesis route is as follows. Formula: C6F13I
Cooled to -78 C. zirconocene dichloride(Cp 2 ZrCl 2, 70.2 mg, 0.24 mmol)Of ether (2.4 mL)To the solution was added n-propylmagnesium chloride (2.0 M in ether solution, 0.12 mL, 0.24 mmol)1,4-Dioxane (23 [mu] L, 0.27 mmol)And n-tridecafluorohexyl iodide (C 6 F 13 I, 78 muL, 0.36 mmol) were added,And the mixture was stirred at the same temperature for 1 hour.Then,Methylaluminoxane(10% toluene solution, 0.16 mL, 0.24 mmol) was added thereto, the temperature was raised to 0 C., and the mixture was stirred for 2 minutes. After adding styrene oxide (23 muL, 0.20 mmol) to this, the temperature was raised to room temperature and stirred for 1 hour.After completion of the reaction, 1 N hydrochloric acid was added to quench the reaction and then extracted 3 times with ether, and the organic layers were combinedDried over sodium sulfate, filtered and the solvent was distilled off under reduced pressure to give a crude product. The crude product obtainedThe product was purified by silica gel column chromatography (hexane / ethyl acetate = 20/1 (v / v)) To obtain 3,3,4,4,5,5,6,6,7,7,8,8,8-tridecaFluoro-1-phenyl-2-hydroxyoctane (77.5 mg, yield: 88%).
The synthetic route of 355-43-1 has been constantly updated, and we look forward to future research findings.
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