Diethyl Ether → HCID 67227223, Verbindung

HRID 573042

Reaktionsgleichung

Reaktionsgleichung von HRID 573042
F[C:2]1[CH:12]=[C:11]([F:13])[CH:10]=[CH:9][C:3]=1[C:4]([O:6][CH2:7][CH3:8])=[O:5].[O-]P([O-])([O-])=O.[K+].[K+].[K+].[CH3:22][C:23]1[NH:24][C:25]2[C:30]([CH:31]=1)=[CH:29][C:28]([OH:32])=[CH:27][CH:26]=2.CCOCC>COCCOCCOC>[F:13][C:11]1[CH:10]=[CH:9][C:3]([C:4]([O:6][CH2:7][CH3:8])=[O:5])=[C:2]([O:32][C:28]2[CH:29]=[C:30]3[C:25](=[CH:26][CH:27]=2)[NH:24][C:23]([CH3:22])=[CH:31]3)[CH:12]=1

Komponenten

6

Edukt 4

HCID 3283Diethyl EtherHCID 62657Potassium Phosphate, TribasicHCID 833362-methyl-1H-indol-5-olHCID 2737170Benzoic acid, 2,4-difluoro-, ethyl ester

Produkt 1

HCID 67227223HCID 67227223, Verbindung

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 8150DiglymeLösungsmittel

Versuchsvorschrift

Ethyl 2,4-difluorobenzoate (1.14 g), K3PO4 (1.30 g) and 2-methyl-5-indolol (0.90 g) were stirred at 110° C. in diglyme (12 mL) for 24 hours. The mixture was cooled and poured into ether. The solution was washed three times with 1M NaOH solution, and with brine, and dried. The solution was then concentrated. The concentrate was chromatographed on silica gel with 10% ethyl acetate/hexanes.

Aufarbeitung

  1. temperatureThe mixture was cooled
  2. washThe solution was washed three times with 1M NaOH solution
  3. dry with materialwith brine, and dried
  4. concentrationThe solution was then concentrated
  5. customThe concentrate was chromatographed on silica gel with 10% ethyl acetate/hexanes

Quellen und Nachweise

ORD-Eintrag
ord-1ee6f62c08ad4d0db339638b3a8d1d3c
Quelldatensatz
uspto-grants-2015_05
Patentnummer
US09029404B2

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