反应详情

A mixture of 2-bromo-4-pyridinecarboxamide (1.1 g), BTPC (35 mg), copper (I) iodide (8 mg), 6-[(6-bromohexyl)oxy]-1-hexyne (1.43 g) and dicyclohexylamine (1.2 ml) in acetonitrile (20 ml) was stirred at room temperature, under nitrogen, for 20 h, then left to stand for 24 h. The yellow mixture was diluted with ether (50 ml), filtered, the filtrate dried and evaporated in vacuo to give a yellow waxy solid. The solid was purified by FCC eluting with System A (98:2:1) to give a pale yellow waxy solid. The solid was dissolved in ethanol:toluene (1:1), (20 ml) treated with activated charcoal (0.2 g), heated, filtered through hyflo and evaporated in vacuo to give the title compound as a pale yellow waxy solid (1.04 g), t.l.c. (toluene-ethanol: 0.880 ammonia, 90:10:1) Rf 0.31.

1. waitleft
2. waitto stand for 24 h
3. filtrationfiltered
4. customthe filtrate dried
5. customevaporated in vacuo
6. customto give a yellow waxy solid
7. customThe solid was purified by FCC
8. washeluting with System A (98:2:1)
9. customto give a pale yellow waxy solid
10. temperatureheated
11. filtrationfiltered through hyflo
12. customevaporated in vacuo