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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
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HRID 1608899 반응식
[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]
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참가 물질

3

반응물 1

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

생성물 1

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

시약·촉매·용매 1

HCID 14797Potassium Hydroxide용매

실험 절차

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.

후처리

  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

출처 및 근거

ORD 기록
ord-7567f8a0c6b8440395cd69dcb5947865
출처 데이터셋
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05399291

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