反应详情

温度

60 °C

Add dropwise isopropylzinc solution (ZnCl2 1M in Et2O (10.5 ml) and isopropylzinc 2M in THF (10.5 ml) previously mixed at 10° C. under N2 atmosphere) to a mechanically stirring suspension of 4-cyano-3-(4-iodo-phenyl)-5-methylsulfanyl-thiophene-2-carboxylic acid ethyl ester (1.5 gr, 3.5 mmol) and 1,3-bis-(diphenylphosphino)propane nickel (II) chloride (380 mg, 0.71 mmol) in dry THF (35 ml) and heat the resulting mixture 60° C. for 1 hour. Cool the reaction to room temperature and remove solvents in vacuo. Purify the solid by chromatography on silica gel (eluting with 10-80% Ethyl acetate/hexane) to provide the title compound in 25% yield: Mass spectrum (EI+): m/z 426 (M++1).

1. additionpreviously mixed at 10° C. under N2 atmosphere) to
2. temperatureCool
3. customthe reaction to room temperature
4. customremove solvents in vacuo
5. customPurify the solid by chromatography on silica gel (eluting with 10-80% Ethyl acetate/hexane)