Реакция #62805

Уравнение реакции

(±)-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

Растворители

1,2-dichloroethane

Условия реакции

Обработка

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

Методика

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.

Источник