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ChemicalBook CAS DataBase List Perfluorooctyl iodide
507-63-1

Perfluorooctyl iodide synthesis

10synthesis methods
-

Yield:-

Reaction Conditions:

Stage #1: perfluorooctyl sulfofluorurewith sodium tetrahydroborate in tetrahydrofuran at 20; for 2 h;
Stage #2: with sulfuryl dichloride in tetrahydrofuran at 20; for 0.5 h;
Stage #3: with potassium iodide in tetrahydrofuran;water at 80; for 2 h;Reflux;

Steps:

1 Example 1

In a 250mL open beaker containing a stir bar, add 100mL of THF solution, weigh 1.14g (0.03mol) of sodium borohydride and add it; adjust the rotor speed to about 800 rpm (too low speed will cause foam to affect the reaction effect),Load 15g (0.03mol) of the sulfonyl fluoride raw material represented by formula (IV-1) on an automatic jet pump of a 10mL syringe; at room temperature, adjust to drip into the system at a dropping rate of 40mL / h. After the addition was completed, the reaction was carried out at room temperature for 2 hours.After the completion of the fluorine spectrum detection reaction, SO2Cl2 (0.06 mol) was added and the reaction was performed at room temperature for 30 minutes. The fluorine spectrum detection reaction was complete. Subsequently, 50 mL of water was added for washing, and then 5 g of KI was added for reaction, and the mixture was heated to 80 ° C. and refluxed for 2 h.The solvent tetrahydrofuran was distilled off to obtain perfluorooctyl iodide represented by the formula (I-1). The total yield was 75% and the purity was> 92%.

References:

CN110759805,2020,A Location in patent:Paragraph 0086-0088

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