反应详情

A mixture of 10-oxo-10H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carboxylic acid (2.5 g, 0.01 mol) and 1,1'-carbonyldiimidazole (1.7 g, 0.01 mol) in dimethylformamide (25 ml) is heated at 90°-95° C. for one hour under nitrogen. The solution is cooled in an ice bath and anhydrous ammonia is bubbled through for 15 minutes. The mixture is stirred at ice bath temperature for 2 hours and at room temperature for one hour. The reaction mixture is cooled and the precipitate is filtered off. The precipitate is washed with tetrahydrofuran and recrystallized from dimethylformamide to give the product (1.2 g.), mp 319°-320° C.

1. temperatureis heated at 90°-95° C. for one hour under nitrogen
2. temperatureThe solution is cooled in an ice bath
3. customanhydrous ammonia is bubbled through for 15 minutes
4. waitat room temperature for one hour
5. temperatureThe reaction mixture is cooled
6. filtrationthe precipitate is filtered off
7. washThe precipitate is washed with tetrahydrofuran
8. customrecrystallized from dimethylformamide
9. customto give the product (1.2 g.), mp 319°-320° C.