反应详情

To a mixture of 4-ethynylanisole (700 mg, 5.30 mmol), 4-iodoanisole (1.30 g, 5.55 mmol), (PPh3)2PdCl2 (74.4 mg, 0.106 mmol), and CuI (10.1 mg, 0.053 mmol) in THF (7 ml), diisopropyl amine (1.13 g, 11.1 mmol) was added dropwise under ice cooling under argon atmosphere. After stirring at room temperature for 1 h, water was added, and the mixture was extracted with ethyl acetate. The organic layer was washed with water then saturated brine, dried over sodium sulfate and concentrated. The residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=15/1) to give bis(4-methoxyphenyl)ethyne (95%).

1. additionwas added dropwise under ice cooling under argon atmosphere
2. extractionthe mixture was extracted with ethyl acetate
3. washThe organic layer was washed with water
4. dry with materialsaturated brine, dried over sodium sulfate
5. concentrationconcentrated
6. customThe residue was purified by silica gel column chromatography (eluent: n-hexane/ethyl acetate=15/1)