反应详情

1.6 g (0.0076 mole) of 5,6-dihydro-5-oxopyrazolo[1,5-c]-quinazoline-2-carbonitrile (prepared as described in Example 2), 546 mg of sodium azide (0.0084 mole or 1.1 equivalent) and 449 mg (1.1 equivalent) of ammonium chloride are suspended in dimethylformamide (30 ml) and the mixture is heated at 100° under N2 for 29 hours with stirring. The reaction mixture is cooled and stripped to dryness. The crude product is suspended in water (75 ml) and treated with concentrated HCl (1.5 ml) to pH 2. The mixture is stirred for ~15 minutes and filtered; the precipitates obtained are washed well with water and air-dried to yield: 2.17 g, quantitative crude yield, m.p. 287°-289°.

1. temperaturethe mixture is heated at 100° under N2 for 29 hours
2. temperatureThe reaction mixture is cooled
3. stirringThe mixture is stirred for ~15 minutes
4. filtrationfiltered
5. customthe precipitates obtained
6. washare washed well with water
7. customair-dried to yield: 2.17 g, quantitative crude
8. customyield