反应详情

温度

100 °C

A mixture of 3,10-dihydro-10-oxo-1H-pyrido[1,2-a]thieno[3,2-d]pyrimidine-7-carbonitrile (0.8 g., 0.003 mol), sodium azide (0.8 g., 0.012 mol) and ammonium chloride (0.07 g., 0.013 mol) in dimethylformamide (100 ml) is heated under nitrogen at 100° C. for 18 hours. The reaction mixture is cooled, poured into ice-water (750 ml), acidified with concentrated hydrochloric acid and stirred for one hour. The precipitate is filtered, washed with water and with acetone. Recrystallization from dimethylformamide gives a crystalline product (0.63 g.), mp 297° C. (dec).

1. temperatureThe reaction mixture is cooled
2. filtrationThe precipitate is filtered
3. washwashed with water and with acetone
4. customRecrystallization from dimethylformamide
5. customgives a crystalline product (0.63 g.), mp 297° C. (dec)