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Methyl 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoate → 4-(5-Butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoic acid

HRID 1608899
ノート
印刷プレビュー

反応式

HRID 1608899 の反応式
[CH2:1]([O:5][CH2:6][C:7]([F:27])([F:26])[C:8]([F:25])([F:24])[C:9]([F:23])([F:22])[CH2:10][O:11][C:12]1[CH:21]=[CH:20][C:15]([C:16]([O:18]C)=[O:17])=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH3:4]>[OH-].[K+]>[CH2:1]([O:5][CH2:6][C:7]([F:26])([F:27])[C:8]([F:24])([F:25])[C:9]([F:22])([F:23])[CH2:10][O:11][C:12]1[CH:21]=[CH:20][C:15]([C:16]([OH:18])=[O:17])=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH3:4]
参加物実験手順後処理出典と根拠反応ノート

参加物

3

反応物 1

HCID 20082759Methyl 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoate

生成物 1

HCID 200827564-(5-Butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoic acid

試薬・触媒・溶媒 1

HCID 14797Potassium Hydroxide溶媒

実験手順

Subsequently, the methyl 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoate was heated at reflux with 20 ml of 10% aqueous KOH for 2 hours. The resulting hydrolyzed carboxylate salt reaction product mixture was then cooled to room temperature and was acidified with concentrated (98%) sulfuric acid. The desired fluorinated benzoic acid precipitate was filtered from the aqueous solution and was washed twice with 10 ml aliquots of deionized water. The product was dried in a vacuum oven at 60° C. and a pressure of 0.2 mm Hg (0.2 torr). A total of 9.5 g of the desired 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoic acid was recovered.

後処理

  1. concentrationwith concentrated (98%) sulfuric acid
  2. filtrationThe desired fluorinated benzoic acid precipitate was filtered from the aqueous solution
  3. washwas washed twice with 10 ml aliquots of deionized water
  4. customThe product was dried in a vacuum oven at 60° C.
  5. customA total of 9.5 g of the desired 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)benzoic acid was recovered

出典と根拠

ORDレコード
ord-7567f8a0c6b8440395cd69dcb5947865
出典データセット
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US05399291

反応ノート

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