Perfluoro(methyl vinyl ether) → Potassium 1,1,2-trifluoro-2-(trifluoromethoxy)ethanesulfonate

HRID 553375

반응식

HRID 553375 반응식
O.[S:2]([O-:5])([O-:4])=[O:3].[K+:6].[K+].S(S([O-])=O)([O-])(=O)=O.[K+].[K+].[C:17]([F:26])([O:21][C:22]([F:25])([F:24])[F:23])=[C:18]([F:20])[F:19]>O>[F:19][C:18]([F:20])([S:2]([O-:5])(=[O:4])=[O:3])[CH:17]([F:26])[O:21][C:22]([F:25])([F:24])[F:23].[K+:6]

참가 물질

5

반응물 3

HCID 14474Perfluoro(methyl vinyl ether)HCID 28019Potassium MetabisulfiteHCID 516933Dipotassium;sulfite;hydrate

생성물 1

HCID 87095932Potassium 1,1,2-trifluoro-2-(trifluoromethoxy)ethanesulfonate

시약·촉매·용매 1

HCID 962Water용매

반응 조건

온도
-35 °C

실험 절차

A 1-gallon Hastelloy C276 reaction vessel is charged with a solution of 114 g potassium sulfite hydrate (KHSO3.H2O, 95%, Aldrich, 0.72 mol), 440 g potassium metabisulfite (K2S2O5, 99%, Mallinckrodt, 1.98 mol) and 2000 mL of deionized water. The pH of this solution is 5.8. The vessel is cooled to −35° C., evacuated to −3 psig (81 kPa), and purged with nitrogen. This evacuate/purge cycle is repeated two more times. 600 g perfluoro(methyl vinyl ether) (PMVE, 3.61 mol) is added to the vessel, which is heated to 125° C. at which time the internal pressure is 462 psig (3290 kPa). The reaction temperature is maintained at 125° C. for 6 hr. The pressure drops to 25 psig (275 kPa) at which point the vessel is vented and cooled to 25° C. Once cooled, a white crystalline precipitate of the forms, leaving clear colorless liquid above it (pH=7). 19F NMR of the white solid shows it to be the desired product in high purity (>98%). 19F NMR of the liquid shows a small but detectable amount of the hydration product of Equation (3), above.

후처리

  1. customevacuated to −3 psig (81 kPa)
  2. custompurged with nitrogen
  3. temperatureis heated to 125° C. at which time the internal pressure
  4. temperatureThe reaction temperature is maintained at 125° C. for 6 hr
  5. temperaturecooled to 25° C
  6. temperatureOnce cooled
  7. customa white crystalline precipitate of the forms, leaving clear colorless liquid above it (pH=7)

출처 및 근거

ORD 기록
ord-e26fce7103aa42efa9fa52fcd300cc66
출처 데이터셋
uspto-grants-2011_11
특허 번호
US08048604B2

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