Triethylamine → HCID 11335869, Verbindung

HRID 1062628Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1062628
Br.Br[CH:3]([C:16]1[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=1)[C:4]([C:6]1[CH:11]=[CH:10][C:9]([C:12]([CH3:15])([CH3:14])[CH3:13])=[CH:8][CH:7]=1)=O.[NH2:22][C:23]([NH2:25])=[S:24].C(N(CC)CC)C>C(#N)C>[CH3:13][C:12]([C:9]1[CH:10]=[CH:11][C:6]([C:4]2[N:22]=[C:23]([NH2:25])[S:24][C:3]=2[C:16]2[CH:21]=[CH:20][N:19]=[CH:18][CH:17]=2)=[CH:7][CH:8]=1)([CH3:15])[CH3:14]

Komponenten

5

Edukt 3

HCID 8471TriethylamineHCID 2723790ThioureaHCID 11315915HCID 11315915, Verbindung

Produkt 1

HCID 11335869HCID 11335869, VerbindungAusbeute 70 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 6342AcetonitrileLösungsmittel

Versuchsvorschrift

To a solution of 2-bromo-1-[4-(1,1-dimethylethyl)phenyl]-2-(4-pyridyl)ethanone hydrobromide (5.0 g, 12 mmol) and thiourea (0.95 g, 13 mmol) in acetonitrile (60 mL) was added dropwise triethylamine (1.8 ml, 13 mmol) and the mixture was refluxed for 3 h. The solvent was evaporated under reduced pressure and saturated aqueous sodium hydrogencarbonate solution was added to the residue. The precipitated solid was collected by filtration. The obtained crude crystal was recrystallized from ethanol to give the title compound (2.6 g, 8.4 mmol, yield 69%).

Aufarbeitung

  1. temperaturethe mixture was refluxed for 3 h
  2. customThe solvent was evaporated under reduced pressure and saturated aqueous sodium hydrogencarbonate solution
  3. additionwas added to the residue
  4. filtrationThe precipitated solid was collected by filtration
  5. customThe obtained crude crystal
  6. customwas recrystallized from ethanol

Quellen und Nachweise

ORD-Eintrag
ord-711ccdfc223c4fdd90d91634aade00ed
Quelldatensatz
uspto-grants-2005_11
Patentnummer
US06962933B1

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