Carbon Dioxide → 1,1,1,2,4,4,5,5,6,6,6-Undecafluoro-2-(trifluoromethyl)-3-hexanone

HRID 986883

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HRID 986883 반응식
[F-:1].[K+].C(=O)=O.[C:6]([C:16](F)=[O:17])([C:9]([C:12]([F:15])([F:14])[F:13])([F:11])[F:10])([F:8])[F:7].[C:19](=[C:22]([C:24]([F:27])([F:26])[F:25])[F:23])([F:21])[F:20]>COCCOCCOC>[F:20][C:19]([F:1])([F:21])[C:22]([F:23])([C:24]([F:27])([F:26])[F:25])[C:16](=[O:17])[C:6]([F:7])([F:8])[C:9]([F:10])([F:11])[C:12]([F:13])([F:14])[F:15]

참가 물질

6

반응물 4

HCID 280Carbon DioxideHCID 8302Hexafluoropropylene3회HCID 67632Heptafluorobutyroyl fluorideHCID 522689Potassium Fluoride

생성물 1

HCID 111430681,1,1,2,4,4,5,5,6,6,6-Undecafluoro-2-(trifluoromethyl)-3-hexanone수율 665.2%

시약·촉매·용매 1

HCID 8150Diglyme용매

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온도
85 °C

실험 절차

Into a clean dry 600 mL Parr reactor equipped with stirrer, heater and thermocouple were added 5.8 g (0.10 mol) of anhydrous potassium fluoride and 108 g of anhydrous diglyme. The contents of the reactor were stirred and cooled with dry ice while 232.5 g (1.02 mol) of n-C3F7COF (approximately 95.0 percent purity) was added to the sealed reactor. The reactor and its contents were then heated, and when a temperature of 72° C. had been reached, 141 g (0.94 mol) of CF2═CFCF3 (hexafluoropropylene) was added at a pressure of 85 psig (5150 torr) over a 3.25 hour time period. During the addition of hexafluoropropylene the temperature of the reactor was increased slowly to 85° C. while maintaining the pressure at less than 90 psig (5400 torr). The pressure at the end of the hexafluoropropylene addition was 40 psig (2800 torr) and did not change over an additional 4-hour hold period. The lower phase was fractionally distilled to give 243.5 grams of 1,1,1,2,4,4,5,5,6,6,6-undecafluoro-2-trifluoromethylhexan-3-one, having a boiling point of 72.5° C. and a purity of 99.9% as determined by gas chromatography. The structure was confirmed by gcms.

후처리

  1. customInto a clean dry 600 mL Parr reactor
  2. customequipped with stirrer
  3. additionwas added to the sealed reactor
  4. temperatureThe reactor and its contents were then heated
  5. customa temperature of 72° C.
  6. temperaturewhile maintaining the pressure at less than 90 psig (5400 torr)
  7. waitdid not change over an additional 4-hour
  8. waithold period
  9. distillationThe lower phase was fractionally distilled

출처 및 근거

ORD 기록
ord-7caaac3f27924953b2d2fde2aac92f49
출처 데이터셋
uspto-grants-2003_10
특허 번호
US06630075B2

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