반응 #62805

반응 방정식

(±)-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

용매

1,2-dichloroethane

반응 조건

후처리

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

실험 절차

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.

출처