反应详情

A mixture of 3,10-dihydro-10-oxo-1H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carboxylic acid (3.0 g., 0.012 mol) and 1,1'-carbonyldiimidazole (2.0 g., 0.012 mol) in tetrahydrofuran (180 ml) and dimethylformamide (3.5 ml) is refluxed under nitrogen for 5 hours. 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 and washed with tetrahydrofuran. The precipitate is treated with hot 0.5 mol aqueous sodium bicarbonate solution, filtered, washed with water, washed with acetone and sucked dry to give the product (2.0 g.), mp 334° C. (dec).

1. temperatureis refluxed under nitrogen for 5 hours
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. washwashed with tetrahydrofuran
8. filtrationfiltered
9. washwashed with water
10. washwashed with acetone
11. customsucked dry
12. customto give the product (2.0 g.), mp 334° C. (dec)