Trifluoroacetic acid → HCID 58042402, Verbindung

HRID 2048116Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 2048116
[Cl:1][C:2]1[C:3]([O:16][C:17]2[CH:18]=[N:19][C:20]([CH:24]3[CH2:26][CH2:25]3)=[C:21]([Cl:23])[CH:22]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([O:9]C(C)(C)C)=[O:8].FC(F)(F)C(O)=O>ClCCl>[Cl:1][C:2]1[C:3]([O:16][C:17]2[CH:18]=[N:19][C:20]([CH:24]3[CH2:25][CH2:26]3)=[C:21]([Cl:23])[CH:22]=2)=[CH:4][C:5]([F:15])=[C:6]([CH:14]=1)[C:7]([OH:9])=[O:8]

Komponenten

4

Edukt 2

HCID 6422Trifluoroacetic acidHCID 58042480HCID 58042480, Verbindung

Produkt 1

HCID 58042402HCID 58042402, VerbindungAusbeute 97 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel

Reaktionsbedingungen

Temperatur
45 °C

Versuchsvorschrift

To a solution of tert-butyl 5-chloro-4-[(5-chloro-6-cyclopropylpyridin-3-yl)oxy]-2-fluorobenzoate (Preparation 264, 54.0 g, 135.59 mmol) in dichloromethane (270 mL) was added trifluoroacetic acid (30.76 mL, 406.77 mmol). The resulting solution was heated at 45° C. for 24 hours and concentrated under reduced pressure at 45° C. tert Butyl methyl ether (100 mL) was added to the residue and the resulting slurry stirred at room temperature for 2.5 hours, filtered, washed with tert butyl methyl ether (20 mL) and dried to give the title compound as an off-white solid (45.0 g, 97%).

Aufarbeitung

  1. concentrationconcentrated under reduced pressure at 45° C. tert Butyl methyl ether (100 mL)
  2. additionwas added to the residue
  3. filtrationfiltered
  4. washwashed with tert butyl methyl ether (20 mL)
  5. customdried

Quellen und Nachweise

ORD-Eintrag
ord-6aa7c4dcabb942ceb29551a63a210785
Quelldatensatz
uspto-grants-2013_11
Patentnummer
US08592629B2

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