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4-(Decyloxy)benzoic acid → 4-(5-Butoxy-2,2,3,3,4,4-hexafluoropentoxy)phenyl 4-decyloxybenzoate

HRID 1608902
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HRID 1608902 반응식
[CH2:1]([O:11][C:12]1[CH:20]=[CH:19][C:15]([C:16]([OH:18])=[O:17])=[CH:14][CH:13]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10].[CH2:21]([O:25][CH2:26][C:27]([F:44])([F:43])[C:28]([F:42])([F:41])[C:29]([F:40])([F:39])[CH2:30][O:31][C:32]1[CH:37]=[CH:36][C:35](O)=[CH:34][CH:33]=1)[CH2:22][CH2:23][CH3:24]>C(Cl)Cl.CN(C1C=CN=CC=1)C>[CH2:1]([O:11][C:12]1[CH:13]=[CH:14][C:15]([C:16]([O:18][C:35]2[CH:34]=[CH:33][C:32]([O:31][CH2:30][C:29]([F:39])([F:40])[C:28]([F:42])([F:41])[C:27]([F:43])([F:44])[CH2:26][O:25][CH2:21][CH2:22][CH2:23][CH3:24])=[CH:37][CH:36]=2)=[O:17])=[CH:19][CH:20]=1)[CH2:2][CH2:3][CH2:4][CH2:5][CH2:6][CH2:7][CH2:8][CH2:9][CH3:10]
참가 물질실험 절차후처리출처 및 근거반응 노트

참가 물질

5

반응물 2

HCID 1385274-(Decyloxy)benzoic acidHCID 200827634-(5-Butoxy-2,2,3,3,4,4-hexafluoropentoxy)phenol

생성물 1

HCID 200827514-(5-Butoxy-2,2,3,3,4,4-hexafluoropentoxy)phenyl 4-decyloxybenzoate수율 12.1%

시약·촉매·용매 2

HCID 142844-(Dimethylamino)pyridine촉매HCID 6344Dichloromethane용매

실험 절차

0.45 g (0.0016 moles) of 4-decyloxybenzoic acid and 0.58 g (0.0016 moles) of 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)phenol (prepared essentially as in Example 5) were dissolved in 25 ml of methylene chloride. N,N-dicyclohexylcarbodiimide (0.35 g, 0.0017 moles) was added to the reaction mixture, followed by 0.05 g of 4-(N,N-dimethylamino)pyridine. The resultant mixture was stirred at room temperature under nitrogen for 18 hours. The resulting urea precipitate was removed from the product solution by filtration, and the filtrate was concentrated on a rotary evaporator at reduced pressure. The crude product was purified by flash chromatography on silica gel (chloroform) to yield 0.12 g of 4-(5-butoxy-2,2,3,3,4,4-hexafluoropentoxy)phenyl 4-decyloxybenzoate.

후처리

  1. customThe resulting urea precipitate was removed from the product solution by filtration
  2. concentrationthe filtrate was concentrated on a rotary evaporator at reduced pressure
  3. customThe crude product was purified by flash chromatography on silica gel (chloroform)

출처 및 근거

ORD 기록
ord-b90baab25ce34140820eaa526c210927
출처 데이터셋
uspto-grants-1995_03
DOI
10.6084/m9.figshare.5104873.v1
특허 번호
US05399291

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