反应详情

A mixture of 3,10-dihydro-10-oxo-1H-pyrido[1,2-a]thieno[3,4-d]pyrimidine-7-carbonitrile (1.0 g., 0.004 mol), sodium azide (0.81 g., 0.012 mol) and ammonium chloride (0.69 g., 0.013 mol) in dimethylformamide (150 ml) is heated at 100°-105° C. for 18 hours. The solvent is removed at reduced pressure. The residue is triturated with 1 N hydrochloric acid, filtered, washed with water, dissolved in 10% aqueous potassium carbonate, filtered and reprecipitated with 1 N hydrochloric acid. The solid is filtered off and recrystallized from dimethylformamide-methanol to give a crystalline product (0.96 g.), mp 285° C.

1. temperatureis heated at 100°-105° C. for 18 hours
2. customThe solvent is removed at reduced pressure
3. customThe residue is triturated with 1 N hydrochloric acid
4. filtrationfiltered
5. washwashed with water
6. dissolutiondissolved in 10% aqueous potassium carbonate
7. filtrationfiltered
8. customreprecipitated with 1 N hydrochloric acid
9. filtrationThe solid is filtered off
10. customrecrystallized from dimethylformamide-methanol
11. customto give a crystalline product (0.96 g.), mp 285° C.