反应详情

温度

50 °C

A solution (0.1 M) of ethyl 5-bromo-4-[(tert-butoxycarbonyl)amino]thiophene-2-carboxylate in THF was treated with trimethylsilylacetylene (1.3 eq.), Et3N (1.5 eq.), CuI (0.04 eq.) and PdCl2(PPh3)2 (0.01 eq.). The solution was heated at 50° C. for 3 h. After cooling down, it was filtered through a pad of celite and washed with AcOEt. The organic layer was washed with brine and dried then concentrated and the residue was purified by flash chromatography on silica gel (1:19 AcOEt/petroleum ether) to afford the title compound (70%) as a solid.

1. temperatureAfter cooling down
2. filtrationit was filtered through a pad of celite
3. washwashed with AcOEt
4. washThe organic layer was washed with brine
5. customdried
6. concentrationthen concentrated
7. customthe residue was purified by flash chromatography on silica gel (1:19 AcOEt/petroleum ether)