Potassium Carbonate → HCID 58433490, Verbindung

HRID 1798956Notizen

Reaktionsgleichung

Reaktionsgleichung von HRID 1798956
[C:1]1([C:7]2(NC)[CH2:12][CH2:11][CH2:10][CH2:9][CH2:8]2)[CH:6]=[CH:5][CH:4]=[CH:3][CH:2]=1.Cl[C:16]1[C:21]([Cl:22])=[CH:20][C:19]([C:23]([F:26])([F:25])[F:24])=[CH:18][N:17]=1.C(=O)([O-])[O-].[K+].[K+].[CH3:33][N:34]1C(=O)CCC1>>[Cl:22][C:21]1[C:16]([NH:34][CH2:33][C:7]2([C:1]3[CH:2]=[CH:3][CH:4]=[CH:5][CH:6]=3)[CH2:8][CH2:9][CH2:10][CH2:11][CH2:12]2)=[N:17][CH:18]=[C:19]([C:23]([F:26])([F:25])[F:24])[CH:20]=1

Komponenten

5

Edukt 4

HCID 11430Potassium CarbonateHCID 13387N-methyl-2-pyrrolidoneHCID 1122342,3-Dichloro-5-(trifluoromethyl)pyridineHCID 262910N-Methyl-1-phenylcyclohexanamine

Produkt 1

HCID 58433490HCID 58433490, Verbindung

Versuchsvorschrift

was prepared from 475 mg of 1-phenyl-cyclohexyl-methylamine by reaction with 596 mg of 2,3-dichloro-5-trifluoromethyl-pyridine in the presence of 354 mg potassium carbonate in 2.5 ml of NMP at 80° C. for 1 hour. After dilution with 20 ml of water, the product was extracted with 30 ml of ethyl acetate and purified by chromatography on silica gel with the eluents dichloromethane:methanol=98:2 to obtain 469 mg g of a light yellow oil.

Aufarbeitung

  1. extractionAfter dilution with 20 ml of water, the product was extracted with 30 ml of ethyl acetate
  2. custompurified by chromatography on silica gel with the eluents dichloromethane
  3. custommethanol=98:2 to obtain 469 mg g of a light yellow oil

Quellen und Nachweise

ORD-Eintrag
ord-9bf982e80f6d48d8aa002d8d0c53d794
Quelldatensatz
uspto-grants-2013_01
Patentnummer
US08344004B2

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