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

HRID 1608902
ノート
印刷プレビュー

反応式

HRID 1608902 の反応式
[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]
参加物実験手順後処理出典と根拠反応ノート

参加物

5

反応物 2

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

生成物 1

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

試薬・触媒・溶媒 2

HCID 142844-(Dimethylamino)pyridine触媒HCID 6344Dichloromethane溶媒

実験手順

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.

後処理

  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)

出典と根拠

ORDレコード
ord-b90baab25ce34140820eaa526c210927
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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