Reaktion #49822

Reaktionsgleichung

N-[2-Cyano-3-(1,4-dihydro-1-phenyl-indeno[1,2-c]pyrazol-3-yl) -3-oxo-propanoyl]-glycine, methyl ester

→

N-[2-cyano-3-(1,4-dihydro 1-phenyl-indeno[1,2-c]pyrazol-3-yl)-3-oxo-propanoyl]-glycine

Ausbeute 73.1%

Lösungsmittel

ethanol

KOH

ethanol

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturheated
2. 2
   TemperaturAfter cooling the precipitate
3. 3
   Filtrationis filtered
4. 4
   Waschenwashed with ethanol
5. 5
   workup.DISSOLUTIONdissolved in water
6. 6
   ExtraktionThe aqueous basic solution is extracted with ethyl acetate
7. 7
   ExtraktionThe precipitate is extracted with ethyl acetate
8. 8
   Waschenthe organic solution washed with N HCl
9. 9
   SonstigeEvaporation to dryness in vacuo
10. 10
    Sonstigegives a residue which

Vorschrift

N-[2-Cyano-3-(1,4-dihydro-1-phenyl-indeno[1,2-c]pyrazol-3-yl) -3-oxo-propanoyl]-glycine, methyl ester (1.7 g), is suspended in 1% KOH solution in 95% ethanol (60 ml) and heated under stirring at the reflux temperature for 30 minutes. After cooling the precipitate is filtered and washed with ethanol, then dissolved in water. The aqueous basic solution is extracted with ethyl acetate and then acidified to pH 3 with 2N HCl. The precipitate is extracted with ethyl acetate and the organic solution washed with N HCl and then with water until neutral. Evaporation to dryness in vacuo gives a residue which is crumbled with ethanol to yield 1.2 g of N-[2-cyano-3-(1,4-dihydro 1-phenyl-indeno[1,2-c]pyrazol-3-yl)-3-oxo-propanoyl]-glycine, m.p. 247°-249° C. dec.

Quelle