Hexafluoropropylene → HCID 131729307, 화합물

HRID 656717노트

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HRID 656717 반응식
FCC(F)(F)C(F)(F)O.[C:10]([CH:17]([O:19][CH2:20][C:21]([C:24]([F:27])([F:26])[F:25])([F:23])[F:22])[OH:18])([C:13]([F:16])([F:15])[F:14])([F:12])[F:11].C(=O)([O-])[O-].[K+].[K+].[F:34][C:35]([F:42])([F:41])[C:36]([F:40])=[C:37]([F:39])[F:38].C(C(COC(C(C(F)(F)F)F)(F)F)(F)F)(F)(F)F>O.C(#N)C>[C:10]([CH:17]([O:18][C:37]([CH:36]([C:35]([F:42])([F:41])[F:34])[F:40])([F:39])[F:38])[O:19][CH2:20][C:21]([C:24]([F:25])([F:26])[F:27])([F:22])[F:23])([C:13]([F:16])([F:15])[F:14])([F:12])[F:11]

참가 물질

8

반응물 5

HCID 8302HexafluoropropyleneHCID 11430Potassium CarbonateHCID 16878528302-70-72회HCID 27785191H,1H,2'H-Perfluorodipropyl etherHCID 713784112,2,3,3,3-Pentafluoro-1-(2,2,3,3,3-pentafluoropropoxy)propan-1-ol

생성물 1

HCID 131729307HCID 131729307, 화합물

시약·촉매·용매 2

HCID 962Water용매HCID 6342Acetonitrile용매

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온도
40 °C

실험 절차

The entire contents of the pentafluoropropanol solution (containing the desired C2F5CH(OH)OCH2C2F5) were placed in a 600 mL Parr reaction vessel along with acetonitrile (167 g) and powdered potassium carbonate (2.9 g). The reactor was sealed, evacuated and heated to 40° C. Hexafluoropropene (64.8 g, 0.43 mole) was added in portions over about two hours and the reactor then held at temperature overnight. The reaction mixture was worked up by pouring into water and washing the resulting lower phase three times with water followed by distillation. The distillation afford a main fraction of boiling point 142° C. The product identity was confirmed by GC-MS and H-1 and F-19 NMR as a mixture of diastereomers in a ratio of 55/45%. One diastereomeric fraction was thought to contain SS and RR enantiomers and the other SR and RS enantiomers. The NMR data showed that the product contained about 4.2% olefin [—OCF═CFCF3] as a 43/57% cis/trans mixture. The excess pentafluoropropanol was converted to CF3CF2CH2OCF2CFHCF3 which was removed during the distillation.

후처리

  1. customThe reactor was sealed
  2. customevacuated
  3. customthen held at temperature overnight
  4. washwashing the resulting lower phase three times with water
  5. distillationfollowed by distillation
  6. distillationThe distillation
  7. customafford a main fraction of boiling point 142° C
  8. customwas removed during the distillation

출처 및 근거

ORD 기록
ord-c6270098ba2b4cc7bed52f03596adf3c
출처 데이터셋
uspto-grants-2011_12
특허 번호
US08071816B2

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