Potassium Carbonate → HCID 178418772, Verbindung

HRID 1586395

Reaktionsgleichung

Reaktionsgleichung von HRID 1586395
[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

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-32b6ef4ac89347b6bfda88317fa4416c
Quelldatensatz
uspto-grants-1999_08
Patentnummer
US05945426

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