Trifluoroacetyl fluoride → 3,3-Difluoro-3-pentafluoroethoxy-2-trifluoromethylpropene

HRID 2106075ノート

反応式

HRID 2106075 の反応式
[F:1][C:2]([F:7])([F:6])[C:3]([F:5])=[O:4].[F-:8].[K+].[CH2:10]=[C:11]([C:16](OS(F)(=O)=O)([F:18])[F:17])[C:12]([F:15])([F:14])[F:13]>COCCOCCOC>[F:17][C:16]([F:18])([O:4][C:3]([F:8])([F:5])[C:2]([F:7])([F:6])[F:1])[C:11]([C:12]([F:15])([F:14])[F:13])=[CH2:10]

参加物

5

反応物 3

HCID 67716Trifluoroacetyl fluorideHCID 522689Potassium FluorideHCID 87741755CH2=C(CF3)CF2Oso2F

生成物 1

HCID 858876563,3-Difluoro-3-pentafluoroethoxy-2-trifluoromethylpropene収率 31%

試薬・触媒・溶媒 1

HCID 8150Diglyme溶媒

反応条件

温度
20 °C

実験手順

Trifluoroacetyl fluoride (6 g, 0.051 mole) is bubbled into a mixture of KF (2.4 g, 0.041 mole) and dry diglyme (15 ml). The reaction mixture is stirred at 20° C. for 30 minutes and then CH2═C(CF3)CF2OSO2F (10 g, 0.041 mile) is added gradually. The resulting mixture is stirred at 20° C. for 1 hour. Hexafluoroisobutylene is distilled from the reaction mixture and the residue is poured into water. The organic layer. is separated, washed in turn with aqueous sodium bicarbonate solution and water, and then dried over MgSO4. Distillation gives 3,3-Difluoro-3-pentafluoroethoxy-2-trifluoromethylpropene (CH2═C(CF3)CF2OCF2CF3) (3.5 g, 31% yield, b.pt. 67° C.).

後処理

  1. stirringThe resulting mixture is stirred at 20° C. for 1 hour
  2. distillationHexafluoroisobutylene is distilled from the reaction mixture
  3. additionthe residue is poured into water
  4. customis separated
  5. washwashed in turn with aqueous sodium bicarbonate solution and water
  6. dry with materialdried over MgSO4
  7. distillationDistillation

出典と根拠

ORDレコード
ord-b5dac57fbe4e4c0e92e0af8d0007ae02
出典データセット
uspto-grants-2009_08
特許番号
US07579499B2

反応ノート

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