Oxygen → 5H-Octafluoropentanoic acid

HRID 2407648

反応式

HRID 2407648 の反応式
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]

参加物

7

反応物 5

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

生成物 1

HCID 1202275H-Octafluoropentanoic acid収率 55.4%

試薬・触媒・溶媒 1

HCID 176Acetic Acid溶媒

反応条件

温度
60 °C

実験手順

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%.

後処理

  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

出典と根拠

ORDレコード
ord-a55f45991a464080aae0c3f82217b00d
出典データセット
uspto-grants-2014_08
特許番号
US08809580B2

関連ノート

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