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Pyridine → 4-Fluorobenzamide

HRID 1826704
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 1826704
[N:1]1C=CC=C(OC2C=C(C=C(C#N)C=2)N)C=1.N1C=CC=CC=1.[F:23][C:24]1[CH:32]=[CH:31][C:27]([C:28](Cl)=[O:29])=[CH:26][CH:25]=1>C(Cl)Cl>[F:23][C:24]1[CH:32]=[CH:31][C:27]([C:28]([NH2:1])=[O:29])=[CH:26][CH:25]=1
KomponentenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

5

Edukt 3

HCID 1049PyridineHCID 678794-Fluorobenzoyl chlorideHCID 22136195HCID 22136195, Verbindung

Produkt 1

HCID 715724-Fluorobenzamide

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6344DichloromethaneLösungsmittel2×

Versuchsvorschrift

Formula I where R1 is Pyridin-3-yl, R2 is CN, and R3 is 4-Fluorophenyl To a solution of 1 eq. ( 0.1 g, 0.473 mmol) of 3-(pyridin-3-yloxy)-5-cyano-aniline in 0.47 M in CH2Cl2 (1 mL) and 1.6 eq. of pyridine (0.56 g, 0.71 mmol) was added 3 eq. of 4-fluorobenzoyl chloride (0.225 g, 1.42 mmol) and the resultant mixture stirred at rt overnight. The reaction mixture was diluted with CH2Cl2, washed with sat. NaHCO3, dried (Na2SO4) and concentrated in vacuo. The resultant residue was diluted with toluene and concentrated in vacuo (5 times). Purification by chromatography over silica with 5% MeOH/CH2Cl2 as the eluant afforded 134 mg of a the desired title compound of Formula I, N-[3-cyano-5-(pyridin-3-yloxy)-phenyl]]-4-fluoro-benzamide, as a solid (85% yield). Mpt 169–172° C. MS (M−1) 332.3.

Aufarbeitung

  1. washwashed with sat. NaHCO3
  2. dry with materialdried (Na2SO4)
  3. concentrationconcentrated in vacuo
  4. additionThe resultant residue was diluted with toluene
  5. concentrationconcentrated in vacuo (5 times)
  6. customPurification by chromatography over silica with 5% MeOH/CH2Cl2 as the eluant

Quellen und Nachweise

ORD-Eintrag
ord-2f7169e922ee42b19bd21418c16f21db
Quelldatensatz
uspto-grants-2006_05
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07053094B2

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