Hexafluoropropylene → C3F7Ochfcf2OC2H4ocf2cfhcf3

HRID 1993149노트

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HRID 1993149 반응식
[C:1]([O:11][CH:12]([C:14]([O:17][CH2:18][CH2:19][OH:20])([F:16])[F:15])[F:13])([C:4]([C:7]([F:10])([F:9])[F:8])([F:6])[F:5])([F:3])[F:2].C(=O)([O-])[O-].[K+].[K+].[F:27][C:28]([F:35])([F:34])[C:29]([F:33])=[C:30]([F:32])[F:31]>C(#N)C>[C:1]([O:11][CH:12]([C:14]([O:17][CH2:18][CH2:19][O:20][C:30]([CH:29]([C:28]([F:35])([F:34])[F:27])[F:33])([F:32])[F:31])([F:16])[F:15])[F:13])([C:4]([C:7]([F:9])([F:8])[F:10])([F:6])[F:5])([F:3])[F:2]

참가 물질

5

반응물 3

HCID 8302HexafluoropropyleneHCID 11430Potassium CarbonateHCID 85908837HCID 85908837, 화합물2회

생성물 1

HCID 21902260C3F7Ochfcf2OC2H4ocf2cfhcf3수율 86.3%

시약·촉매·용매 1

HCID 6342Acetonitrile용매

반응 조건

온도
30 °C

실험 절차

Perfluoropropylvinyl ether (139.0 g, 0.52 mole), potassium carbonate (19.3 g, 0.14 mole), ethylene glycol (155.5 g, 2.5 mole) and acetonitrile (200 mL) were combined in a 600 mL Parr reactor. The reactor was sealed and heated to 30° C. for 2.75 hours. The reaction mixture was filtered and then water washed four times to give 146.4 g of C3F7OCFHCF2OC2H4OH (54.2%) and (C3F7OCFHCF2OCH2)2 (43.4%). This material was combined with 179 g from a previous run consisting of 21.6% C3F7OCFHCF2OC2H4OH and 76.1% (C3F7OCFHCF2OCH2)2 and fractionated to give a 106.3 g fractionation cut boiling from 167-173° C. of C3F7OCFHCF2OC2H4OH (80.8% pure). This material along with potassium carbonate (7.3 g, 0.052 mole) and acetonitrile (200 mL) were added to a 600 mL Parr reactor. The reactor was sealed and heated to 30° C. Hexafluoropropene (48.5 g, 0.32 mole) was added to the reactor over a 30 minute period and the reactor contents were held at 30° C. an additional 40 minutes. The reactor was cooled and the contents filtered into a 1-L separatory funnel and water washed four times, dried with anhydrous sodium sulfate and filtered. The material was shaken with anhydrous HF, water washed, dried with anhydrous sodium sulfate and filtered to give 125.6 g of C3F7OCHFCF2OC2H4OCF2CFHCF3 (86.3% pure). The material was fractionated in the concentric tube unit to give 72.3 g of C3F7OCHFCF2OC2H4OCF2CFHCF3 (95.3% purity) boiling at 194° C. Structure was confirmed by gc-ms. The viscosity was 48 centistokes (48×10−6 m2/s) at −50° C. measured using a Cannon-Fenske viscometer and a Wescan Model 221 viscosity timer.

후처리

  1. customto give a 106.3 g fractionation cut
  2. customThe reactor was sealed
  3. temperatureThe reactor was cooled
  4. filtrationthe contents filtered into a 1-L separatory funnel
  5. washwater washed four times
  6. dry with materialdried with anhydrous sodium sulfate
  7. filtrationfiltered
  8. washwashed
  9. dry with materialdried with anhydrous sodium sulfate
  10. filtrationfiltered

출처 및 근거

ORD 기록
ord-3d5436cb72bd4977876183e4f3c73297
출처 데이터셋
uspto-grants-2010_01
특허 번호
US07651627B2

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