Reaktion #62805

Reaktionsgleichung

(±)-3,4,5,8-tetrahydro-7-methyl-5-(3-nitrophenyl)-4-oxo-pyrido[2,3-d]-pyrimidine-6-carboxylic acid isopropyl ester

trimethyloxonium tetrafluoroborate

→

(±)-5,8-Dihydro-4-methoxy-7-methyl-5-(3-nitrophenyl)pyrido[2,3-d]pyrimidine-6-carboxylic acid isopropyl ester

Lösungsmittel

1,2-dichloroethane

Reaktionsbedingungen

Aufarbeitung

1. 1
   ExtraktionThe product is extracted twice with 50 ml saturated sodium hydrogen carbonate solution
2. 2
   Sonstigethe organic phase is separated
3. 3
   Trocknendried over sodium sulfate
4. 4
   SonstigeTwice recrystallizing the residue from diisopropyl ether/isopropanol
5. 5
   Sonstigeyields the product in the form of colorless crystals with a mp of 212°-213° C.

Vorschrift

Three and 0.7 g (10 mmol) (±)-3,4,5,8-tetrahydro-7-methyl-5-(3-nitrophenyl)-4-oxo-pyrido[2,3-d]-pyrimidine-6-carboxylic acid isopropyl ester and 3.0 g (20 mmol) trimethyloxonium-tetrafluoroborate are stirred in 150 ml 1,2-dichloroethane in nitrogen atmosphere and at room temperature for three hours. The product is extracted twice with 50 ml saturated sodium hydrogen carbonate solution, the organic phase is separated, dried over sodium sulfate and reduced under vacuum. Twice recrystallizing the residue from diisopropyl ether/isopropanol yields the product in the form of colorless crystals with a mp of 212°-213° C.

Quelle