反应详情

温度

120 °C

1.57 g (4.5 mmol) of 4-Iodo-5-thiophen-2-yl-2H-pyrazole-3-carboxylic acid ethyl ester, 0.81 g (9.0 mmol) of copper cyanide and 352 mg (2.3 mmol) of tetraethylammonium cyanide were dissolved in 10 ml of DMF and 20 ml of tetrahydrofuran and the solution was degassed with argon. 223 mg (0.2 mmol) of Tris(dibenzylideneacetone)dipalladium (0) and 374 mg (0.7 mmol) of 1,1′-bis-(diphenylphosphino) ferrocene were added at RT. The reaction was stirred at 120° C. for 5 h. The solvent was removed under reduced pressure. The residue was dissolved in ethyl acetate and this solution was washed with saturated aqueous sodium bicarbonate. The organic phase was dried with sodium sulfate, filtered and the solvent was removed under reduced pressure. The product was purified by silica gel chromatography eluting with n-heptane:ethyl acetate/1:1.

1. custom20 ml of tetrahydrofuran and the solution was degassed with argon
2. customThe solvent was removed under reduced pressure
3. dissolutionThe residue was dissolved in ethyl acetate
4. washthis solution was washed with saturated aqueous sodium bicarbonate
5. dry with materialThe organic phase was dried with sodium sulfate
6. filtrationfiltered
7. customthe solvent was removed under reduced pressure
8. customThe product was purified by silica gel chromatography
9. washeluting with n-heptane