反应详情

温度

100 °C

To a stirred solution of phenylacetylene (15.0 μg, 0.137 mmol) and 8a (25.3 mg, 0.0682 mmol) in a mixture of 2 mL of DMF and 1 mL of NEt3, was added Pd(OAc)2 (1.53 mg, 6.82 μmol) and triphenylphosphine (3.57 mg, 13.6 μmol) in a seal tube. The tube was sealed under argon and the mixture was stirred at 100° C. for 18 h. The mixture was cooled and concentrated to dryness in vacuo and the crude product was purified by chromatography on a silica gel column. Elution with n-heptane/EtOAc (2:1) as eluent yielded 13a as a white solid (14 mg, 70%). mp: >300° C. (decomp.),

1. customThe tube was sealed under argon
2. temperatureThe mixture was cooled
3. concentrationconcentrated to dryness in vacuo
4. customthe crude product was purified by chromatography on a silica gel column
5. washElution with n-heptane/EtOAc (2:1) as eluent