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2,2,2-Trifluoroethanol → Ethyl 2,2,2-trifluoroethyl carbonate

HRID 1457378
ノート
印刷プレビュー

反応式

HRID 1457378 の反応式
[F:1][C:2]([F:6])([F:5])[CH2:3][OH:4].[C:7](Cl)(=[O:11])[O:8][CH2:9][CH3:10].[OH-].[K+]>C(OCC)C>[C:7](=[O:11])([O:4][CH2:3][C:2]([F:6])([F:5])[F:1])[O:8][CH2:9][CH3:10]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 3

HCID 64092,2,2-TrifluoroethanolHCID 10928Ethyl chloroformateHCID 14797Potassium Hydroxide

生成物 1

HCID 21263423Ethyl 2,2,2-trifluoroethyl carbonate収率 70%

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

実験手順

In a flask (5-liter volume), 2,2,2-trifluoroethanol (800 g, 8.0 mol), ethyl chlorocarbonate (867 g, 8.0 mol) and diethyl ether (1000 ml) were charged. While the flask was cooled so that the reaction was carried out at -5° C. to 0 ° C., a 29.5% by weight aqueous solution of potassium hydroxide (1500 g) was added dropwise to the flask for 6 hours and the mixture was stirred for 12 hours at room temperature. The ether layer was separated, washed with water, dried and distilled to give ethyl 2,2,2-trifluoroethyl carbonate as a colorless liquid (960 g, yield 70%). The chemical structure of the produced compound was determined based on the IR and NMR absorbance spectra shown in FIG. 5 and FIG. 6 respectively and the mass spectrometry spectrum (M/e=172).

後処理

  1. temperatureWhile the flask was cooled so that the reaction
  2. customwas carried out at -5° C. to 0 ° C.
  3. customThe ether layer was separated
  4. washwashed with water
  5. customdried
  6. distillationdistilled

出典と根拠

ORDレコード
ord-1f57a19fce294e8d92bff3e5a0c67f58
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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