反应详情

A mixture of 2.30 g (7.37 mmol) 2-iodo-5-(4-methoxyphenyl)pyrazine and 1.56 mL (11.1 mmol) ethynyltrimethylsilane in 30 mL THF is charged with 0.12 g (0.15 mmol) bis(triphenylphosphine)dichloropalladium, 0.03 g (15.0 mmol) CuI and 3.01 mL (22.1 mmol) TEA. After stirring at r.t. for 4 h the reaction mixture is diluted with DCM and washed with 50 mL aq. 5% ammonia solution (1×) and 50 mL water (1×). The organic layer is dried with MgSO4 and the solvent is removed in vacuo. The residue is treated with PE/EtOAc (8/2), filtered through a plug of silica gel and the solvent is again removed in vacuo. The product is used without further purification.

1. washwashed with 50 mL aq. 5% ammonia solution (1×) and 50 mL water (1×)
2. dry with materialThe organic layer is dried with MgSO4
3. customthe solvent is removed in vacuo
4. additionThe residue is treated with PE/EtOAc (8/2)
5. filtrationfiltered through a plug of silica gel
6. customthe solvent is again removed in vacuo
7. customThe product is used without further purification