2,2,3,3-Tetrafluorobutane-1,4-diyl bis(trifluoromethanesulfonate) synthesis

Yield:159760-17-5 100%

Reaction Conditions:

Stage #1: 2,2,3,3-tetrafluoro-1,4-butanediolwith pyridine in dichloromethane at 0; for 0.166667 h;
Stage #2: trifluoromethylsulfonic anhydride in dichloromethane at 20; for 12 h;

Steps:

3 Example 3

General procedure: 2,2,3,3-tetrafluoro-1,4-butanediol (4.0000 g, 24.68 mmol) in a 250 mL round bottom flask,2,2,3,3,4,4-hexafluoro-1,5-pentanediol (5.2386 g, 24.68 mmol)Or 2,2,3,3,4,4,5,5-octafluoro-1,6-hexanediol (6.4667 g, 24.68 mmol)Add to 75mL DCM and cool to 0 ° C, then add 5 mL of pyridine and stir for 10 minutes.Then, trifluoromethanesulfonic anhydride (12.5 mL, 74.04 mmol) was slowly added dropwise thereto, and after completion of the dropwise addition, the mixture was warmed to room temperature and stirred for 12 hours.Diluted with DCM, washed with water and saturated brine, dried over anhydrous sodium sulfate and dried.A white solid 4F-OTf, an oil 6F-OTf, and a white solid 8F-OTf were obtained, respectively, yield 100.0%.

References:

CN109776483,2019,A Location in patent:Paragraph 0054-0056