反应详情

A mixture of 1.5 g (0.005 mol) of 4-oxo-2-phenyl-4H-pyrido[1,2-a]thieno[2,3-d]pyrimidine-7-carbonitrile (Example 31), 1.0 g (0.0153 mol) of sodium azide and 0.9 g (0.0168 mol) of ammonium chloride in 200 ml of dimethylformamide is heated at 110°-120° C. for three days. The reaction mixture is cooled, poured into 1 l of ice water and acidified with concentrated hydrochloric acid. The resulting precipitate is filtered and dissolved in hot pyridine, activated charcoal (Darco-G60, Matheson, Coleman and Bell) is added and the hot suspension is filtered through Supercell Hyflo® (Johns-Manville). The filtrate is cooled to give 0.55 g of 2-phenyl-7-(1H-tetrazol-5-yl)-4H-pyrido[1,2-a]thieno[2,3-d]pyrimidin-4-one; mp 310°-312° C. (dec) after recrystallization from pyridine.

1. temperatureis heated at 110°-120° C. for three days
2. temperatureThe reaction mixture is cooled
3. filtrationThe resulting precipitate is filtered
4. dissolutiondissolved in hot pyridine
5. additionactivated charcoal (Darco-G60, Matheson, Coleman and Bell) is added
6. filtrationthe hot suspension is filtered through Supercell Hyflo® (Johns-Manville)
7. temperatureThe filtrate is cooled