Reaktion #702609

Reaktionsgleichung

ethyl 10-chloro-2,3-dihydro-1,3-dimethyl-7-oxo-1H, 7H-pyrido[1,2,3-de]quinoxaline-6-carboxylate

charcoal

→

10-chloro-2,3-dihydro-1,3-dimethyl-7-oxo-1H,7H-pyrido[1,2,3-de]quinoxaline-6-carboxylic acid

Lösungsmittel

sodium hydroxide

Reaktionsbedingungen

Aufarbeitung

1. 1
   Temperaturis heated on a steam bath for five hours
2. 2
   Filtrationfiltered
3. 3
   SonstigeThe product is separated by filtration
4. 4
   Waschenwashed with water
5. 5
   Sonstigerecrystallized from N,N-dimethylformamide

Vorschrift

A mixture of 13.8 g of ethyl 10-chloro-2,3-dihydro-1,3-dimethyl-7-oxo-1H, 7H-pyrido[1,2,3-de]quinoxaline-6-carboxylate and 600 ml of three percent sodium hydroxide solution is heated on a steam bath for five hours. The solution is treated with decolorizing charcoal, filtered and neutralized to pH 7 with acetic acid. The product is separated by filtration, washed with water and recrystallized from N,N-dimethylformamide to provide yellow crystals of 10-chloro-2,3-dihydro-1,3-dimethyl-7-oxo-1H,7H-pyrido[1,2,3-de]quinoxaline-6-carboxylic acid, m.p. 243°-245° C. Analysis: Calculated for C14H13ClN2O3 : %C, 57.5; %H, 4.5; %N, 9.6. Found %C, 58.0; %H, 4.3; %N, 9.7.

Quelle