StartseiteMCPWorkbenchSkills
StartseiteWorkbenchBenachrichtigungenMein Bereich
llms.txt · MCP-AnleitungDatenschutz · Nutzungsbedingungen · Supportv1.8.0
  1. Startseite
  2. /Reaktion

2,4-Dimethylaniline → Aniline

HRID 598056
Notizen
Druckvorschau

Reaktionsgleichung

Reaktionsgleichung von HRID 598056
Br[C:2]1[C:3](=[O:12])[N:4]([CH3:11])[CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1.[CH3:13][C:14]1[CH:20]=[C:19]([CH3:21])[CH:18]=[CH:17][C:15]=1[NH2:16].C1(P(C2C=CC=CC=2)C2C=CC3C(=CC=CC=3)C=2C2C3C(=CC=CC=3)C=CC=2P(C2C=CC=CC=2)C2C=CC=CC=2)C=CC=CC=1.CC(C)([O-])C.[Na+]>C1(C)C=CC=CC=1.C(OCC)(=O)C.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.C1C=CC(/C=C/C(/C=C/C2C=CC=CC=2)=O)=CC=1.[Pd].[Pd]>[CH3:13][C:14]1[CH:20]=[C:19]([CH3:21])[CH:18]=[CH:17][C:15]=1[NH:16][C:2]1[C:3](=[O:12])[N:4]([CH3:11])[CH:5]=[C:6]([N+:8]([O-:10])=[O:9])[CH:7]=1.[NH2:16][C:15]1[CH:17]=[CH:18][CH:19]=[CH:20][CH:14]=1
KomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion

Komponenten

9

Edukt 4

HCID 72502,4-DimethylanilineHCID 634876Binap, (A+-)-HCID 23676156Sodium t-butoxideHCID 672674813-Bromo-1-methyl-5-nitro-2(1H)-pyridinone

Produkt 2

HCID 6115AnilineHCID 672679503-[(2,4-Dimethylphenyl)amino]-1-methyl-5-nitropyridin-2(1H)-one

Reagenzien, Katalysatoren, Lösungsmittel 3

HCID 9811564Bis(dibenzylideneacetone)palladiumKatalysatorHCID 1140TolueneLösungsmittelHCID 8857Ethyl AcetateLösungsmittel

Reaktionsbedingungen

Temperatur
95 °C

Versuchsvorschrift

To a solution containing 0.60 g (2.57 mmol) of 3-bromo-1-methyl-5-nitropyridin-2(1H)-one in 120 ml of toluene under a nitrogen atmosphere was added 0.64 ml (5.15 mmol) of 2,4-dimethylaniline, 1.61 g (2.57 mmol) of rac-2,2′-bis(diphenylphosphino)-1,1′-binaphthyl (racemic BINAP), 0.37 g (3.85 mmol) of sodium t-butoxide and 1.20 g (1.31 mmol) of tris(dibenzylideneacetone)dipalladium (0). The reaction was heated to 95° C. overnight. The reaction was cooled to room temperature, diluted with ethyl acetate and washed with saturated sodium bicarbonate. The organic phase was dried over magnesium sulfate. Filtration, removal of solvent and purification of the residue via biotage eluting with 60% ethyl acetate/hexanes gave the desired product with some starting aniline. The material was triturated with hexanes and the solids filtered and dried to afford 0.154 g (21.9%) of product.

Aufarbeitung

  1. temperatureThe reaction was cooled to room temperature
  2. washwashed with saturated sodium bicarbonate
  3. dry with materialThe organic phase was dried over magnesium sulfate
  4. filtrationFiltration, removal of solvent and purification of the residue via biotage
  5. washeluting with 60% ethyl acetate/hexanes

Quellen und Nachweise

ORD-Eintrag
ord-6f11ef843c1843bf979f4d549fc34825
Quelldatensatz
uspto-grants-2011_03
DOI
10.6084/m9.figshare.5104873.v1
Patentnummer
US07897607B2

Notizen zur Reaktion

Wird geladen…

Auf dieser SeiteKomponentenReaktionsbedingungenVersuchsvorschriftAufarbeitungQuellen und NachweiseNotizen zur Reaktion