Hexafluoroacetone → CH2=C(CF3)CF2Ocf(CF3)2

HRID 1594458ノート

反応式

HRID 1594458 の反応式
[CH2:1]=[C:2]([C:7]([O:10]S(F)(=O)=O)([F:9])[F:8])[C:3]([F:6])([F:5])[F:4].[C:15](O[K])([C:21]([F:24])([F:23])[F:22])([C:17]([F:20])([F:19])[F:18])[F:16].[F-].[K+].FC(F)(F)C(C(F)(F)F)=O>O.COCCOCCOC>[CH2:1]=[C:2]([C:7]([O:10][C:15]([C:21]([F:24])([F:23])[F:22])([C:17]([F:20])([F:19])[F:18])[F:16])([F:9])[F:8])[C:3]([F:6])([F:5])[F:4]

参加物

7

反応物 4

HCID 12695HexafluoroacetoneHCID 522689Potassium FluorideHCID 87741755CH2=C(CF3)CF2Oso2FHCID 178506340HCID 178506340、化合物

生成物 1

HCID 131726622CH2=C(CF3)CF2Ocf(CF3)2収率 75%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8150Diglyme溶媒

実験手順

CH2═C(CF3)CF2OSO2F (10 g, 0.041 mole) is added at 20° C. to (CF3)2CFOK, prepared from freshly dried potassium fluoride (KF) (2.4 g, 0.041 mole), hexafluoroacetone (HFA) (9.3 g, 0.056 mole) and dry diglyme (10 ml). The reaction mixture is agitated for 2 hours and then poured into water, the organic layer separating. The organic layer is washed with dilute hydrochloric acid, then sodium bicarbonate solution, then water, after which it is dried over magnesium sulfate (MgSO4). Distillation of the reaction mixture gives CH2═C(CF3)CF2OCF(CF3)2 (10.2 g, 75% yield, b.pt. 87-88° C.).

後処理

  1. customthe organic layer separating
  2. washThe organic layer is washed with dilute hydrochloric acid
  3. dry with materialsodium bicarbonate solution, then water, after which it is dried over magnesium sulfate (MgSO4)
  4. distillationDistillation of the reaction mixture

出典と根拠

ORDレコード
ord-1ffe82ee73284e6f94c8aa82185afd74
出典データセット
uspto-grants-2007_11
特許番号
US07301059B2

反応ノート

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