反应详情

To a room temperature solution of 4-amino-2-phenylamino-pyrimidine-5-carboxaldehyde (2.89 g, 13.50 mmol) in 120 mL of tetrahydrofuran was added (carbethoxymethylene)triphenylphosphorane (11.00 g, 31.60 mmol). The reaction mixture was heated at reflux for 9 hours then stirred at room temperature overnight. The solution was concentrated in vacuo and treated with ethyl acetate and hexane to give a yellow solid. The solid was collected by filtration and purified by flash chromatography to give 1.55 g (40%) of ethyl 3-(4-amino-2-phenylamino-pyrimidin-5-yl)acrylate, mp 190-192° C.

1. temperatureThe reaction mixture was heated
2. temperatureat reflux for 9 hours
3. concentrationThe solution was concentrated in vacuo
4. additiontreated with ethyl acetate and hexane
5. customto give a yellow solid
6. filtrationThe solid was collected by filtration
7. custompurified by flash chromatography