反应详情

温度

140 °C

A mixture of 0.60 g (1.70 mmol) of the starting material XXIII, 3 ml of dimethylformamide, 0.12 g (1.87 mmol) of sodium azide and 0.10 g (1.87 mmol) of ammonium chloride was stirred at 140° C. for 30 min. The cooled reaction mixture was diluted with water and the precipitated crystals were filtered off. The so obtained product was purified by column chromatography using silica gel (MN Kieselgel 60) as adsorbent and a mixture of chloroform-methanol (99:1) as eluent to yield 0.68 g (54%) of the title compound; Mp.: 263-264° C.

1. customThe cooled reaction mixture
2. filtrationthe precipitated crystals were filtered off
3. customThe so obtained product
4. customwas purified by column chromatography
5. additiona mixture of chloroform-methanol (99:1) as eluent