Sulfur tetrafluoride → Perfluoro-3-(butoxy)propene

HRID 1680424

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HRID 1680424 반응식
[F-:1].[K+].[F:3][C:4]([F:15])([C:11]([F:14])([F:13])[F:12])[C:5]([F:10])([F:9])[C:6]([F:8])=[O:7].S(F)(F)(F)F.S(F)(O[C:25]([F:32])([F:31])[C:26]([F:30])=[C:27]([F:29])[F:28])(=O)=O>COCCOCCOC>[F:28][C:27]([F:29])=[C:26]([F:30])[C:25]([F:32])([F:31])[O:7][C:6]([F:1])([F:8])[C:5]([F:10])([F:9])[C:4]([F:15])([F:3])[C:11]([F:12])([F:13])[F:14]

참가 물질

6

반응물 4

HCID 24555Sulfur tetrafluorideHCID 67632Heptafluorobutyroyl fluorideHCID 522689Potassium FluorideHCID 2776028Pentafluoroallyl fluorosulphate

생성물 1

HCID 54369168Perfluoro-3-(butoxy)propene수율 64%

시약·촉매·용매 1

HCID 8150Diglyme용매

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온도
5 °C

실험 절차

A mixture of dry potassium fluoride (7.50 g, 0.13 mol), diglyme (100 ml) and heptafluorobutyroyl fluoride (prepared from the acid by treatment with sulfur tetrafluoride) (28.1 g, 0.13 mol) was stirred at 5° C. for 30 min. Perfluoroallyl fluorosulfate was added dropwise at 5° C., the mixture was stirred at this temperature for 1 hour, then at 25° C. for 3 hours. The volatile components were transferred by distillation at 40° C. (8 mm Hg), washed with water (100 ml), and distilled from a small amount of concentrated sulfuric acid to give perfluoro-3-(butoxy)propene (30.3 g, 0.083 mol, 64%) bp 80°-84° C. whose structure was confirmed by:

후처리

  1. stirringthe mixture was stirred at this temperature for 1 hour
  2. waitat 25° C. for 3 hours
  3. distillationThe volatile components were transferred by distillation at 40° C. (8 mm Hg)
  4. washwashed with water (100 ml)
  5. distillationdistilled from a small amount of concentrated sulfuric acid

출처 및 근거

ORD 기록
ord-583dc2b02951406291c442ca2545b358
출처 데이터셋
uspto-grants-1981_06
특허 번호
US04273729

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