Difluoro(fluorosulphonyl)acetyl fluoride → CH2=C(CF2Ocf2CF2SO2F)2

HRID 1178841

反応式

HRID 1178841 の反応式
[CH2:1]=[C:2]([C:11](OS(F)(=O)=O)([F:13])[F:12])[C:3]([O:6][S:7]([F:10])(=[O:9])=[O:8])([F:5])[F:4].[F:19][S:20]([C:23]([C:26]([O:29][K])([F:28])[F:27])([F:25])[F:24])(=[O:22])=[O:21].[F-:31].[K+].[F:33][S:34]([C:37]([C:40]([F:42])=[O:41])([F:39])[F:38])(=[O:36])=[O:35]>COCCOCCOC.O>[CH2:1]=[C:2]([C:3]([O:6][S:7]([F:10])(=[O:9])=[O:8])([F:5])[F:4])[C:11]([F:13])([F:19])[F:12].[CH2:1]=[C:2]([C:11]([O:41][C:40]([C:37]([S:34]([F:33])(=[O:36])=[O:35])([F:39])[F:38])([F:31])[F:42])([F:13])[F:12])[C:3]([O:29][C:26]([C:23]([S:20]([F:19])(=[O:22])=[O:21])([F:25])[F:24])([F:28])[F:27])([F:5])[F:4]

参加物

8

反応物 4

HCID 69614Difluoro(fluorosulphonyl)acetyl fluorideHCID 522689Potassium FluorideHCID 10471472CH2=C(CF2Oso2F)2HCID 178527443HCID 178527443、化合物

生成物 2

HCID 87741755CH2=C(CF3)CF2Oso2FHCID 131726625CH2=C(CF2Ocf2CF2SO2F)2収率 58%

試薬・触媒・溶媒 2

HCID 962Water溶媒HCID 8150Diglyme溶媒

反応条件

温度
20 °C

実験手順

CH2═C(CF2OSO2F)2 is added gradually to FSO2CF2CF2OK, which is prepared from freshly dried KF (3.9 g, 0.067 mole) and FSO2CF2COF (12 g, 0.067 mole) in dry diglyme (30 ml). The resulting mixture is stirred 3 hours at 20° C. The reaction mixture is poured into water. The organic layer is washed with aqueous sodium bicarbonate, then water, and then dried over MgSO4. Distillation gives CH2═C(CF3)CF2OSO2F (0.5 g) and CH2═C(CF2OCF2CF2SO2F)2 (9 g, 58% yield, b.pt. 95–96° C. at 15 mm Hg).

後処理

  1. washThe organic layer is washed with aqueous sodium bicarbonate
  2. dry with materialwater, and then dried over MgSO4
  3. distillationDistillation

出典と根拠

ORDレコード
ord-2a360d231027458abc5d04db8e2f8c79
出典データセット
uspto-grants-2007_10
特許番号
US07276624B2

関連ノート

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