反应详情

The title compound from Example 1 (127 mg, 0.25 mmol) was suspended in triethylamine (2 mL) and trimethylsilylacetylene (38 mg, 0.39 mmol) and acetonitrile (2 mL to try and solubilise reactants). Pd(PPh3)2Cl2 (5 mg, 0.006 mmol) and cuprous iodide (1.2 mg, 0.006 mmol) were added and the reaction mixture stirred. After 1 h a further portion of trimethylsilylacetylene (19 mg, 0.19 mmol) was added and stirring continued for 2 h. The solvent was evaporated and the residue partitioned between ethyl acetate and water. The organics were washed with brine, dried (MgSO4) and concentrated to give a brown foam. Purification by flash column chromatography (gradient elution from 100% dichloromethane to 99% dichloromethane/methanol) gave the title compound as a light brown solid (108 mg).

1. stirringstirring
2. customThe solvent was evaporated
3. customthe residue partitioned between ethyl acetate and water
4. washThe organics were washed with brine
5. dry with materialdried (MgSO4)
6. concentrationconcentrated
7. customto give a brown foam
8. customPurification
9. washby flash column chromatography (gradient elution from 100% dichloromethane to 99% dichloromethane/methanol)