反应详情

温度

80 °C

A mixture of ethyl 5-bromo-thiophene-2-carboxylate (500 mg, 2.13 mmol), trimethylsilylacetylene (0.445 mL, 3.2 mmol), Pd(PPh3)4 (15 mg) and CuI (10 mg) in diisopropylamine (10 mL) was heated at 80° C. for 2 h. After being cooled to room temperature, the mixture was filtered through CELITE, and the filtrate was poured into water. The product was extracted with EtOAc. The EtOAc solution was washed with brine, dried over MgSO4, concentrated in vacuo to give ethyl 5-(2-trimethylsilyl-ethyn-1-yl)-thiophene-2-carboxylate (529 mg). MS 253 (M+H).

1. temperatureAfter being cooled to room temperature
2. filtrationthe mixture was filtered through CELITE
3. additionthe filtrate was poured into water
4. extractionThe product was extracted with EtOAc
5. washThe EtOAc solution was washed with brine
6. dry with materialdried over MgSO4
7. concentrationconcentrated in vacuo