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

HRID 1457379
ノート
印刷プレビュー

反応式

HRID 1457379 の反応式
[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]
参加物反応条件実験手順後処理出典と根拠反応ノート

参加物

4

反応物 2

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

生成物 1

HCID 18183634Methyl 2,2,3,3,3-pentafluoropropyl carbonate収率 51%

試薬・触媒・溶媒 1

HCID 23694274Sodium methanolate methanol触媒

反応条件

温度
120 °C

実験手順

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).

後処理

  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

出典と根拠

ORDレコード
ord-3cf89bf823f449cf83da662303b85e4b
出典データセット
uspto-grants-1998_12
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05847188

反応ノート

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