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ChemicalBook CAS DataBase List HEXAFLUOROGLUTARYL CHLORIDE

HEXAFLUOROGLUTARYL CHLORIDE synthesis

4synthesis methods
-

Yield: 84%

Reaction Conditions:

with iron(III) chloride;Benzotrichlorid at 24 - 130;Inert atmosphere;

Steps:

12 Example 12 (Ex-12): Synthesis of 2,2,3,3,4,4-hexafluoropentanedioyl dichloride
Anhydrous perfluoroglutaric acid (20.2 g, 84.1 mmol), made as described above, and anhydrous FcCl·, (210 mg, 1.3 mmol) were placed in a 50 mL three-necked flask equipped with a thermometer and reflux condenser in an inert atmosphere. Then, benzotrichloride (32.5 g, 166.2 mmol) was added. Upon intense stirnng, the reaction mixture was slowly warmed to 40 °C during 2 h, and foam formation was observed. The reaction mixture was stirred 4 h at 130 °C and overnight at 24 °C. The reflux condenser was substituted by a distillation set with a short Vigreux column and the reaction mixture was distilled. The product 2,2,3,3,4,4-hexafluoropentanedioyl dichloride was obtained in 84% yield (19.5 g, 70.4 mmol, b.p. 112-116 °C/760 mmHg).

References:

3M INNOVATIVE PROPERTIES COMPANY;HIRSCHBERG, Markus E.;HINTZER, Klaus;LAMANNA, William M.;SMITH, Sean M.;RÖSCHENTHALER, Gerd-Volker;PAJKERT, Romana;TVERDOMED, Sergey N. WO2019/123342, 2019, A1 Location in patent:Page/Page column 24

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