Oxygen → 5H-Octafluoropentanoic acid

HRID 2407648

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HRID 2407648 반응식
N([O-])=O.[Na+].CC1(C)N([O])C(C)(C)CCC1.CC(O[Na])=[O:18].[F:21][C:22]([F:34])([C:25]([F:33])([F:32])[C:26]([F:31])([F:30])[CH:27]([F:29])[F:28])[CH2:23][OH:24].O=O>C(O)(=O)C>[F:21][C:22]([F:34])([C:25]([F:32])([F:33])[C:26]([F:30])([F:31])[CH:27]([F:28])[F:29])[C:23]([OH:18])=[O:24]

참가 물질

7

반응물 5

HCID 977OxygenHCID 96412,2,3,3,4,4,5,5-Octafluoro-1-pentanolHCID 2724126TempoHCID 23668193Sodium NitriteHCID 178418247HCID 178418247, 화합물

생성물 1

HCID 1202275H-Octafluoropentanoic acid수율 55.4%

시약·촉매·용매 1

HCID 176Acetic Acid용매

반응 조건

온도
60 °C

실험 절차

60 mL of acetic acid, 0.46 g sodium nitrite, TEMPO (0.35 g), CH3CO2Na (6.88 g) and 6.5 g of 2,2,3,3,4,4,5,5-octafluoro-pentan-1-ol were placed in a 100 mL1 glass flask equipped with a balloon containing oxygen, a reflux condenser and a stirrer. The mixture was stirred for 16 hr at 60° C. upon which the mixture was acidified as described in example 17 and extracted with diethyl ether (three times). The combined organic phases were washed with water and dried over magnesium sulfate. The solvent was removed at a rotary evaporator and the residue was distilled to give 3.82 g of acid (20 mmHg, 65° C.). Yield: 55%.

후처리

  1. customequipped with a balloon
  2. extractionextracted with diethyl ether (three times)
  3. washThe combined organic phases were washed with water
  4. dry with materialdried over magnesium sulfate
  5. customThe solvent was removed at a rotary evaporator
  6. distillationthe residue was distilled

출처 및 근거

ORD 기록
ord-a55f45991a464080aae0c3f82217b00d
출처 데이터셋
uspto-grants-2014_08
특허 번호
US08809580B2

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