反应详情

A mixture of 3,10-dihydro-10-oxo-1H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carboxylic acid (4.4 g., 0.018 mol) and 1,1'-carboxyldiimidazole (2.9 g., 0.018 mol) in tetrahydrofuran (300 ml) and dimethylformamide (4 ml) is refluxed under nitrogen for 3.5 hours. The solution is cooled in an ice bath and anhydrous ammonia is bubbled through for 45 minutes. The precipitate is filtered off, washed with hot 0.5 M. aqueous sodium bicarbonate solution, with hot dimethylformamide with ether and dried to give a yellow powder (2.9 g.). mp 285° C. (dec).

1. temperatureis refluxed under nitrogen for 3.5 hours
2. temperatureThe solution is cooled in an ice bath
3. customanhydrous ammonia is bubbled through for 45 minutes
4. filtrationThe precipitate is filtered off
5. washwashed with hot 0.5 M
6. dry with materialaqueous sodium bicarbonate solution, with hot dimethylformamide with ether and dried
7. customto give a yellow powder (2.9 g.)