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Water → 5,5,6,6,6-Pentafluorohexanoic acid

HRID 1267736
ノート
印刷プレビュー

反応式

HRID 1267736 の反応式
S(=O)(=O)(O)[OH:2].[F:6][C:7]([F:18])([C:14]([F:17])([F:16])[F:15])[CH2:8][CH2:9][CH2:10][CH2:11]C#N.[OH2:19]>>[F:6][C:7]([F:18])([C:14]([F:17])([F:16])[F:15])[CH2:8][CH2:9][CH2:10][C:11]([OH:2])=[O:19]
参加物実験手順後処理出典と根拠反応ノート

参加物

4

反応物 3

HCID 962Water2 回HCID 1118Sulfuric AcidHCID 185462625,5,6,6,6-Pentafluorohexanecarbonitrile

生成物 1

HCID 120170595,5,6,6,6-Pentafluorohexanoic acid収率 85%

実験手順

Concentrated sulfuric acid (350 ml) was slowly added dropwise to 5,5,6,6,6-pentafluorohexanecarbonitrile (108 g, 577.20 mmol) at 0° C., and the resulting mixture was stirred for 3 hours at room temperature. Water (350 ml) was slowly added dropwise to this mixture at 0° C., followed by heating under reflux for 12 hours. After cooling to room temperature, water was added to the reaction mixture, which was then extracted three times with dichloromethane. The combined organic layers were washed with water and saturated aqueous sodium chloride, and then dried over anhydrous magnesium sulfate. The solvent was distilled off to give 5,5,6,6,6-pentafluorohexanoic acid (95.8 g, Yield 85%).

後処理

  1. temperatureby heating
  2. temperatureunder reflux for 12 hours
  3. temperatureAfter cooling to room temperature
  4. extractionwas then extracted three times with dichloromethane
  5. washThe combined organic layers were washed with water and saturated aqueous sodium chloride
  6. dry with materialdried over anhydrous magnesium sulfate
  7. distillationThe solvent was distilled off

出典と根拠

ORDレコード
ord-016e3135ea034b8c9aac70eef6b191a5
出典データセット
uspto-grants-2003_04
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US06552068B1

反応ノート

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