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2,2,3,3,3-Pentafluoropropanol → Methyl 2,2,3,3,3-pentafluoropropyl carbonate

HRID 2258149
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HRID 2258149 반응식
[F:1][C:2]([F:9])([C:5]([F:8])([F:7])[F:6])[CH2:3][OH:4].[C:10](=O)([O:13]C)[O:11][CH3:12]>C[O-].[Na+].CO>[C:10](=[O:13])([O:4][CH2:3][C:2]([F:9])([F:1])[C:5]([F:8])([F:7])[F:6])[O:11][CH3:12]
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참가 물질

4

반응물 2

HCID 98722,2,3,3,3-PentafluoropropanolHCID 12021Dimethyl Carbonate

생성물 1

HCID 18183634Methyl 2,2,3,3,3-pentafluoropropyl carbonate수율 51%

시약·촉매·용매 1

HCID 23694274Sodium methanolate methanol촉매

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온도
120 °C

실험 절차

In a flask (500-ml volume) equipped with 10 distillation columns, 2,2,3,3,3-pentafluoropropanol (100 g, 0.67 mol), dimethyl carbonate (180 g, 2.0 mol) and a 28% sodium methoxide/methanol solution (1.3 g) were charged. The flask was heated to 120° C. to allow the starting materials to react for 10 hours while removing the methanol from the distillation columns by evaporation. After allowing the mixture to cool to room temperature, an aqueous solution of ammonium chloride was added to the mixture and the mixture was shaken to remove the sodium methoxide. The organic layer was washed with water, dried and distilled to give methyl 2,2,3,3,3-pentafluoropropyl carbonate as a colorless liquid (71 g, yield 51%). The chemical structure of the produced compound was determined based on the IR and NMR absorbance spectra shown in FIG. 7 and FIG. 8 respectively and the mass spectrometry spectrum (M/e=208).

후처리

  1. customto react for 10 hours
  2. customwhile removing the methanol
  3. distillationfrom the distillation columns
  4. customby evaporation
  5. temperatureto cool to room temperature
  6. additionan aqueous solution of ammonium chloride was added to the mixture
  7. customto remove the sodium methoxide
  8. washThe organic layer was washed with water
  9. customdried
  10. distillationdistilled

출처 및 근거

ORD 기록
ord-fd726fd74ea243348808b6096a4907b5
출처 데이터셋
uspto-grants-1997_08
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05659062

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