反应详情

(1H-indazol-3-ylmethyl)triphenylphosphonium iodide (3.20 g, 6.15 mmol) obtained in Step 4 was dissolved in methanol (60 mL), and the solution was added with methyl p-formylbenzoate (1.00 g, 6.09 mmol) and potassium carbonate (2.55 g, 18.5 mmol), followed by stirring at room temperature overnight. The reaction mixture was added with water, and was extracted with ethyl acetate, then the organic layer was washed with saturated brine, and was dried over anhydrous sodium sulfate, and the solvent was evaporated under reduced pressure. The residue was purified by thin-layer chromatography (chloroform/methanol=15/1), was further triturated in mixed solvent of ethyl acetate/diisopropyl ether to obtain methyl (E)-4-[2-(1H-indazol-3-yl)vinyl]benzoate (0.87 g, 51%).

1. extractionwas extracted with ethyl acetate
2. washthe organic layer was washed with saturated brine
3. dry with materialwas dried over anhydrous sodium sulfate
4. customthe solvent was evaporated under reduced pressure
5. customThe residue was purified by thin-layer chromatography (chloroform/methanol=15/1)
6. customwas further triturated in mixed solvent of ethyl acetate/diisopropyl ether