反应详情

Na2CO3 (146 mg, 1.37 mmol) was added to a stirred solution of 4-iodo-1-trityl-1H-pyrazole (300 mg, 0.69 mmol) in toluene: H2O (5:1, 11.5 mL). Pd (PPh3)4 (80 mg, 0.07 mmol) and phenylboronic acid (126 mg, 1.03 mmol) were then added and the reaction mixture was heated to reflux for 2 hrs. The reaction mixture was then diluted with water and the product was extracted with ethyl acetate. The organic layer was washed with saturated brine solution, dried over sodium sulphate and concentrated to get the residue. The residue obtained was purified by column chromatography (using silica gel of 60-120 mesh and 5% EtOAc in Hexane as eluent) afford 120 mg (48.38% yield) of 4-phenyl-1-trityl-1H-pyrazole. 1H NMR (CDCl3): δ 7.96-7.94 (s, 1H), 7.64-7.6 (s, 1H), 7.46-7.4 (d, 2H), 7.36-7.0 (m, 1H), 7.24-7.16 (m, 7H).

1. temperaturethe reaction mixture was heated
2. temperatureto reflux for 2 hrs
3. extractionthe product was extracted with ethyl acetate
4. washThe organic layer was washed with saturated brine solution
5. dry with materialdried over sodium sulphate
6. concentrationconcentrated
7. customto get the residue
8. customThe residue obtained
9. customwas purified by column chromatography (using silica gel of 60-120 mesh and 5% EtOAc in Hexane as eluent)