反応 #62805

反応方程式

(±)-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

溶媒

1,2-dichloroethane

反応条件

後処理

1. 1
   抽出The product is extracted twice with 50 ml saturated sodium hydrogen carbonate solution
2. 2
   その他the organic phase is separated
3. 3
   乾燥dried over sodium sulfate
4. 4
   その他Twice recrystallizing the residue from diisopropyl ether/isopropanol
5. 5
   その他yields the product in the form of colorless crystals with a mp of 212°-213° C.

実験手順

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.

出典