Trifluoroacetic acid → 2-[(2,5-Dichloropyridin-3-yl)oxy]-2-methylpropionic acid

HRID 1026539Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1026539
[Cl:1][C:2]1[C:7]([O:8][C:9]([CH3:18])([CH3:17])[C:10]([O:12]C(C)(C)C)=[O:11])=[CH:6][C:5]([Cl:19])=[CH:4][N:3]=1.FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:7]([O:8][C:9]([CH3:17])([CH3:18])[C:10]([OH:12])=[O:11])=[CH:6][C:5]([Cl:19])=[CH:4][N:3]=1

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 86671386Tert-butyl 2-[(2,5-dichloropyridin-3-yl)oxy]-2-methylpropionate

Produkt 1

HCID 866713872-[(2,5-Dichloropyridin-3-yl)oxy]-2-methylpropionic acidAusbeute 125,5 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Versuchsvorschrift

To a dichloromethane solution (157 ml) of tert-butyl 2-[(2,5-dichloropyridin-3-yl)oxy]-2-methylpropionate (79.1 g) was added at 0° C. trifluoroacetic acid (157 ml). The reaction solution was brought back to room temperature, stirred overnight, and then concentrated under reduced pressure. The residue was dissolved in ethyl acetate, washed sequentially with water and saturated sodium chloride solution, dried over anhydrous sodium sulfate, and concentrated under reduced pressure. The residue was azeotroped with toluene to afford 2-[(2,5-dichloropyridin-3-yl)oxy]-2-methylpropionic acid (81.1 g).

Aufarbeitung

  1. customwas brought back to room temperature
  2. concentrationconcentrated under reduced pressure
  3. dissolutionThe residue was dissolved in ethyl acetate
  4. washwashed sequentially with water and saturated sodium chloride solution
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationconcentrated under reduced pressure
  7. customThe residue was azeotroped with toluene

Quellen und Nachweise

ORD-Eintrag
ord-0b56ff09ed5144dda50816a792bad4d0
Quelldatensatz
uspto-grants-2014_05
Patentnummer
US08729095B2

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