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

HRID 1091991노트

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HRID 1091991 반응식
[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]

참가 물질

5

반응물 3

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

생성물 1

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

시약·촉매·용매 1

HCID 3283Diethyl Ether용매

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온도
0 °C

실험 절차

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).

후처리

  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

출처 및 근거

ORD 기록
ord-659e35fab9084018bab185a9d10f4178
출처 데이터셋
uspto-grants-2012_03
특허 번호
US08129412B2

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