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Water → N-(2-(2-chlorophenyl)-4-oxo-1,4-dihydro-1,7-naphthyridin-6-yl)cyclopropanecarboxamide

HRID 468846
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Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 468846
Cl[C:2]1[CH:3]=[C:4]2[C:9](=[CH:10][N:11]=1)[NH:8][C:7]([C:12]1[CH:17]=[CH:16][CH:15]=[CH:14][C:13]=1[Cl:18])=[CH:6][C:5]2=[O:19].[CH:20]1([C:23]([NH2:25])=[O:24])[CH2:22][CH2:21]1.C(=O)([O-])[O-].[Cs+].[Cs+].O>O1CCOCC1.[Cl-].[Na+].O>[Cl:18][C:13]1[CH:14]=[CH:15][CH:16]=[CH:17][C:12]=1[C:7]1[NH:8][C:9]2[C:4]([C:5](=[O:19])[CH:6]=1)=[CH:3][C:2]([NH:25][C:23]([CH:20]1[CH2:22][CH2:21]1)=[O:24])=[N:11][CH:10]=2
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Komponenten

7

Edukt 4

HCID 962WaterHCID 10796Cesium carbonateHCID 80376Cyclopropanecarboxamide2×HCID 866749476-chloro-2-(2-chlorophenyl)-1,7-naphthyridin-4(1H)-one

Produkt 1

HCID 67977259N-(2-(2-chlorophenyl)-4-oxo-1,4-dihydro-1,7-naphthyridin-6-yl)cyclopropanecarboxamideAusbeute 6,2 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 312751,4-DioxaneLösungsmittelHCID 57417360Sodium chloride; waterLösungsmittel

Versuchsvorschrift

A mixture of 6-chloro-2-(2-chlorophenyl)-1,7-naphthyridin-4(1H)-one (29.2 mg, 100 μmol), cyclopropanecarboxamide (17.1 mg, 200 μmol), chloro[2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl][2-(2-aminoeth yl)phenyl]palladium(II) (8.0 mg, 10 μmol), 2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl (5.4 mg, 10 μmol), and cesium carbonate (98.0 mg, 301 μmol) in 1,4-dioxane (5.0 mL) was heated to reflux for 4 hours. Further portions of cyclopropanecarboxamide (17.1 mg, 200 μmol), chloro[2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl][2-(2-aminoeth yl)phenyl]palladium(II) (8.0 mg, 10 μmol) and 2-(dicyclohexylphosphino)-3,6-dimethoxy-2′-4′-6′-tri-1-propyl-1,1′-biphenyl (5.4 mg, 10 μmol) were added and the mixture heated to reflux for 16 hours. The cooled mixture was treated with water and brine and extracted with ethyl acetate, and the separated organic phase washed with brine, dried over sodium sulfate, filtered, and concentrated in vacuo. The residue was purified by reverse phase HPLC (gradient of acetonitrile in water with 0.1% formic acid) to afford the title compound as a white solid (2.1 mg, 6.2%). LCMS (Method E): RT=3.715 min, M+H+=340.0 & 342.0.

Aufarbeitung

  1. temperaturewas heated
  2. temperatureto reflux for 4 hours
  3. temperaturethe mixture heated
  4. temperatureto reflux for 16 hours
  5. extractionextracted with ethyl acetate
  6. washthe separated organic phase washed with brine
  7. dry with materialdried over sodium sulfate
  8. filtrationfiltered
  9. concentrationconcentrated in vacuo
  10. customThe residue was purified by reverse phase HPLC (gradient of acetonitrile in water with 0.1% formic acid)

Quellen und Nachweise

ORD-Eintrag
ord-ec2c039f7a5f43f89bb96ebc222bfb74
Quelldatensatz
uspto-grants-2014_01
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US08623889B2

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