Potassium Carbonate → HCID 178418772, Verbindung

HRID 635888

Reaktionsgleichung

Reaktionsgleichung von HRID 635888
[F:1][C:2]1[CH:7]=[CH:6][C:5]([C:8](=O)[CH2:9][C:10]([O:12]CC)=O)=[CH:4][CH:3]=1.Cl.[C:17]([NH2:20])(=[NH:19])[CH3:18].C(=O)([O-])[O-].[K+].[K+]>C(O)C>[F:1][C:2]1[CH:3]=[CH:4][C:5]([C:8]2[CH:9]=[C:10]([OH:12])[N:20]=[C:17]([CH3:18])[N:19]=2)=[CH:6][CH:7]=1

Komponenten

5

Edukt 3

HCID 11430Potassium CarbonateHCID 67170Acetamidine monohydrochlorideHCID 2758844Ethyl 3-(4-Fluorophenyl)-3-Oxopropanoate

Produkt 1

HCID 178418772HCID 178418772, VerbindungAusbeute 63 %

Reagenzien, Katalysatoren, Lösungsmittel 1

HCID 702EthanolLösungsmittel

Reaktionsbedingungen

Temperatur
65 °C

Versuchsvorschrift

(Step 2) A mixture of 145 g of ethyl 3-(4-fluorophenyl)-3-oxopropionate, 97.8 g of acetamidine hydrochloride, 191 g of powdered potassium carbonate, and 1.16 L of ethanol was stirred at 60-70° C. for 16 hours. This reaction mixture was filtered to remove insolubles and the filtrate was concentrated. To the residue was added water and the resultant was neutralized with acetic acid. The crystals that separated out were collected by filtration, washed with water, and dried to provide 88.7 g of the title compound as white crystals. m.p. 290-292° C. (decomp.)

Aufarbeitung

  1. filtrationThis reaction mixture was filtered
  2. customto remove insolubles
  3. concentrationthe filtrate was concentrated
  4. additionTo the residue was added water
  5. customThe crystals that separated out
  6. filtrationwere collected by filtration
  7. washwashed with water
  8. customdried

Quellen und Nachweise

ORD-Eintrag
ord-066fe036f2d443f8863dc2f44abb0f3f
Quelldatensatz
uspto-grants-2001_02
Patentnummer
US06191149B1

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