2,2,3,3,3-Pentafluoropropanol → 2,2,3,3,3-Pentafluoropropyl nonafluorobutane-1-sulfonate

HRID 1091991ノート

反応式

HRID 1091991 の反応式
[F:1][C:2]([F:9])([C:5]([F:8])([F:7])[F:6])[CH2:3][OH:4].[H-].[Na+].[F:12][C:13]([F:28])([S:24](F)(=[O:26])=[O:25])[C:14]([F:23])([F:22])[C:15]([F:21])([F:20])[C:16]([F:19])([F:18])[F:17]>CCOCC>[F:1][C:2]([F:9])([C:5]([F:8])([F:7])[F:6])[CH2:3][O:4][S:24]([C:13]([F:12])([F:28])[C:14]([F:22])([F:23])[C:15]([F:20])([F:21])[C:16]([F:19])([F:18])[F:17])(=[O:26])=[O:25]

参加物

5

反応物 3

HCID 98722,2,3,3,3-PentafluoropropanolHCID 24758Sodium hydrideHCID 67814Perfluoro-1-butanesulfonyl fluoride

生成物 1

HCID 866246582,2,3,3,3-Pentafluoropropyl nonafluorobutane-1-sulfonate

試薬・触媒・溶媒 1

HCID 3283Diethyl Ether溶媒

反応条件

温度
0 °C

実験手順

2,2,3,3,3-pentafluoropropanol (3.0 g) was added to a suspension of sodium hydride (1.08 g) in dry ether (50 ml) at 0° C. under an argon atmosphere. Stirred at 0° C. for 15 minutes. Perfluoro-1-butanesulphonyl fluoride (12.08 g) was slowly added. Stirred at reflux for 3 hours, cooled and carefully quenched with H2O. Extracted with ether, twice. The combined extracts were washed with saturated brine dried over MgSO4, filtered and evaporated to give 2,2,3,3,3-pentafluoropropyl-1,1,2,2,3,3,4,4,4-nonafluorobutane-1-sulphonate as an oil. Yield 7.9 g. NMR: (CDCl3) δ 4.9 (m, 2H).

後処理

  1. stirringStirred
  2. temperatureat reflux for 3 hours
  3. temperaturecooled
  4. customcarefully quenched with H2O
  5. extractionExtracted with ether
  6. washThe combined extracts were washed with saturated brine
  7. dry with materialdried over MgSO4
  8. filtrationfiltered
  9. customevaporated

出典と根拠

ORDレコード
ord-659e35fab9084018bab185a9d10f4178
出典データセット
uspto-grants-2012_03
特許番号
US08129412B2

反応ノート

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