Diethyl Malonate → HCID 178489012, Verbindung

HRID 2412538

Reaktionsgleichung

Reaktionsgleichung von HRID 2412538
C[O-].[Na+].Cl.[CH3:5][O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]([NH2:13])=[NH:12])=[CH:9][CH:8]=1.[C:16](OCC)(=[O:23])[CH2:17][C:18](OCC)=[O:19]>CO.C(O)C>[CH3:5][O:6][C:7]1[CH:15]=[CH:14][C:10]([C:11]2[N:13]=[C:18]([OH:19])[CH:17]=[C:16]([OH:23])[N:12]=2)=[CH:9][CH:8]=1

Komponenten

6

Edukt 3

HCID 7761Diethyl MalonateHCID 10942334Sodium MethoxideHCID 123262194-Methoxybenzamidine Hydrochloride

Produkt 1

HCID 178489012HCID 178489012, VerbindungAusbeute 83,9 %

Reagenzien, Katalysatoren, Lösungsmittel 2

HCID 702EthanolLösungsmittelHCID 887MethanolLösungsmittel

Versuchsvorschrift

338 g of a 30% solution of sodium methylate in methanol are added over 10 minutes to a suspension of 112 g of p-methoxybenzamidine hydrochloride and 101 g of diethyl malonate in 520 ml of ethanol, and the mixture is subsequently refluxed for 5 hours. The reaction mixture is then concentrated by rotary evaporation and the residue is dissolved in 1000 ml of warm water of 80° C. The solution is filtered and the filtrate is acidified to pH 1. The precipitate is isolated by filtration and vacuum dried at 80° C., affording 109.8 g of 2-p-methoxyphenyl-4,6-dihydroxypyrimidine with a melting point of 318° C. (decompos.).

Aufarbeitung

  1. temperaturethe mixture is subsequently refluxed for 5 hours
  2. concentrationThe reaction mixture is then concentrated by rotary evaporation
  3. dissolutionthe residue is dissolved in 1000 ml of warm water of 80° C
  4. filtrationThe solution is filtered
  5. customThe precipitate is isolated by filtration and vacuum
  6. customdried at 80° C.

Quellen und Nachweise

ORD-Eintrag
ord-ca44de7b2bd24bf59f5a86a5629e9eaf
Quelldatensatz
uspto-grants-1985_01
Patentnummer
US04493726

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