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

HRID 1178834ノート

反応式

HRID 1178834 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-1a3de0f532f4482eb5a079a83273e2c0
出典データセット
uspto-grants-2007_10
特許番号
US07276624B2

反応ノート

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