反应详情

A screw-top Schlenk flask (250 mL) purged with dry nitrogen was charged with compound 25B (7.31 g, 40 mmol) and 4-chlorophenylacetylene (5.0 g, 36.6 mmol). At room temperature, degassed 1,2-dichloroethane (100 mL) was added followed by [Cp*RuCl(cod)] (450 mg, 1.18 mmol) and triethylamine (6.38 mL, 45.8 mmol). The flask was purged with N2 and capped. After being stirred at room temperature for 7 h, the reaction mixture was passed through a plug of silica gel, and washed with DCM. The resulting solution was concentrated and the residue was purified by column chromatography on silica gel (pure hexanes to 10:1 hexanes/EtOAc) to provide the desired compound. MS (m/z) 282.0 [M+H]+.

1. customA screw-top Schlenk flask (250 mL) purged with dry nitrogen
2. customAt room temperature, degassed 1,2-dichloroethane (100 mL)
3. additionwas added
4. customThe flask was purged with N2
5. customcapped
6. washwashed with DCM
7. concentrationThe resulting solution was concentrated
8. customthe residue was purified by column chromatography on silica gel (pure hexanes to 10:1 hexanes/EtOAc)