反应详情

温度

110 °C

A mixture of 3-methyl-4-oxo-4H,5H-[1]benzothiopyrano[4,3-b]pyran-2-carbonitrile (3.14 g, 12.3 mmoles, described in Example 6), sodium azide (0.884 g, 13.6 mmoles) and ammonium chloride (0.130 g, 2.4 mmoles) in dimethylformamide (18 ml) is heated at 110° C. for 18 hr. The dark solution is evaporated and the residue is dissolved in water (50 ml). The aqueous solution is washed with ethyl acetate and acidified with 10% hydrochloric acid. The precipitate is collected, washed with water and crystallized from acetone-water to give the title compound (2.5 g), mp 247°-248° C.

1. customThe dark solution is evaporated
2. dissolutionthe residue is dissolved in water (50 ml)
3. washThe aqueous solution is washed with ethyl acetate
4. customThe precipitate is collected
5. washwashed with water
6. customcrystallized from acetone-water