Potassium Carbonate → HCID 66811056, Verbindung

HRID 1097383Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1097383
[CH:1]1[C:12]2=[C:13]3[CH:8]([CH2:9][CH2:10][CH2:11]2)[CH2:7][CH2:6][CH2:5][C:4]3=[CH:3][C:2]=1[NH2:14].Cl[C:16]1[N:21]=[CH:20][C:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:18][N:17]=1.C(=O)([O-])[O-].[K+].[K+]>O>[CH:1]1[C:12]2=[C:13]3[CH:8]([CH2:9][CH2:10][CH2:11]2)[CH2:7][CH2:6][CH2:5][C:4]3=[CH:3][C:2]=1[NH:14][C:16]1[N:17]=[CH:18][C:19]([C:22]([O:24][CH2:25][CH3:26])=[O:23])=[CH:20][N:21]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 104878152-Chloro-pyrimidine-5-carboxylic acid ethyl esterHCID 58420580HCID 58420580, Verbindung

Produkt 1

HCID 66811056HCID 66811056, VerbindungAusbeute 93 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 962WaterLösungsmittel

Reaktionsbedingungen

Temperatur
110 °C

Versuchsvorschrift

5,6,6a,7,8,9-Hexahydro-4H-2-phenalenylamine (0.100 g) was added with ethyl 2-chloropyrimidine-5-carboxylate (0.101 g) and potassium carbonate (0.400 g), and the mixture was stirred overnight at 110° C. The reaction mixture was left to cool and then added with water, and the mixture was extracted with chloroform. The organic layer was washed successively with water and saturated brine, and dried over anhydrous sodium sulfate. The organic layer was concentrated under reduced pressure, and the resulting residue was purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:20) to obtain the title compound (0.167 g, yield: 93%).

Aufarbeitung

  1. waitThe reaction mixture was left
  2. temperatureto cool
  3. extractionthe mixture was extracted with chloroform
  4. washThe organic layer was washed successively with water and saturated brine
  5. dry with materialdried over anhydrous sodium sulfate
  6. concentrationThe organic layer was concentrated under reduced pressure
  7. customthe resulting residue was purified by silica gel column chromatography (developing solvent: ethyl acetate:n-hexane=1:20)

Quellen und Nachweise

ORD-Eintrag
ord-c75edd88428b404ead5e0490a17bfa5e
Quelldatensatz
uspto-grants-2012_03
Patentnummer
US08143260B2

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