反应详情

A mixture of 2-[3-[(6-bromohexyl)oxy]-1-propynyl]-5-nitropyridine (5 g) and dipotassium azodicarboxylate (30 g) in pyridine (200 ml) was stirred at room temperature, and acetic acid (18 ml) added. The mixture was stirred overnight and evaporated in vacuo to give a residue oil which was partitioned between 8% sodium bicarbonate (20 ml) and ethyl acetate (20 ml). The organic phase was dried and concentrated to give an oil which was purified by FCC eluting with hexane-ether (1:2→methanol) to give the title compound as an orange oil (300 mg), t.l.c. (toluene:ethanol 0.88 ammonia 80:20:1) Rf 0.75.

1. stirringThe mixture was stirred overnight
2. customevaporated in vacuo
3. customto give a residue oil which
4. customwas partitioned between 8% sodium bicarbonate (20 ml) and ethyl acetate (20 ml)
5. customThe organic phase was dried
6. concentrationconcentrated
7. customto give an oil which
8. customwas purified by FCC
9. washeluting with hexane-ether (1:2→methanol)