Tetrahydrofuran → Potassium 1,1,2,2-tetrafluoro-2-(pentafluoroethoxy)ethane-1-sulfonate

HRID 3952

反応式

HRID 3952 の反応式
[F:1][C:2]([F:18])([S:14](F)(=[O:16])=[O:15])[C:3]([F:13])([F:12])[O:4][C:5]([F:11])([F:10])[C:6]([F:9])([F:8])[F:7].C[Si](C)(C)[O-:21].[K+:24].O1CCCC1>OCC(CO)O>[F:1][C:2]([F:18])([S:14]([O-:21])(=[O:16])=[O:15])[C:3]([F:13])([F:12])[O:4][C:5]([F:11])([F:10])[C:6]([F:9])([F:8])[F:7].[K+:24]

参加物

5

反応物 3

HCID 8028TetrahydrofuranHCID 27825671,1,2,2-tetrafluoro-2-(1,1,2,2,2-pentafluoroethoxy)ethanesulfonyl FluorideHCID 23668039Potassium trimethylsilanolate

生成物 1

HCID 2782415Potassium 1,1,2,2-tetrafluoro-2-(pentafluoroethoxy)ethane-1-sulfonate収率 65%

試薬・触媒・溶媒 1

HCID 753Glycerol溶媒

実験手順

The procedure of Example 1 was followed using perfluoro-3-oxapentanesulfonyl fluoride (7.95 g, 25 mmol), potassium trimethylsilanolate (3.2 g, 25 mmol) and dry tetrahydrofuran (100 mL) while heating at reflux for 1.5 h. Potassium perfluoro-3-oxapentanesulfonate (3.79 g initially and 1.74 g by concentrating the filtrate under vacuum; total 5.53 g, 65% yield) was isolated as a white solid: 19F NMR (fluorotrichloromethane) δ -79.4 (m, CF2, 2F), -83.2 (s, CF3, 3F), -84.9 (m, CF2, 2F), -115.0 ppm (m, CF2, 2F); Positive ion Fast Atom Bombardment MS (Glycerol matrix, Cs⊕ ion bombardment) m/e 393, 747, 1101, 1455, 1809 for M+K⊕ to M5 +K⊕.

後処理

  1. temperaturewhile heating
  2. temperatureat reflux for 1.5 h
  3. concentrationPotassium perfluoro-3-oxapentanesulfonate (3.79 g initially and 1.74 g by concentrating the filtrate under vacuum
  4. customtotal 5.53 g, 65% yield) was isolated as a white solid

出典と根拠

ORDレコード
ord-bced94d3b141486e89edeb33840b194b
出典データセット
uspto-grants-1988_02
特許番号
US04723016

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