反应详情

Into an oven dried flask containing magnesium turnings (0.408 g, 17 mmol) and tetrahydrofuran (10 ml) was added 3-bromoanisole (3.1 g, 17 mmol )and the reaction mixture was heated at reflux. After 2 h, the reaction mixture was cooled to room temperature and 5-amino-1-(4-fluorophenyl)-4-(2-pyridylthiocarboxy)pyrazole (1.5 g, 4.8 mmol) was added and the stirring was continued for 1 h. The reaction mixture was quenched with water and the product was extracted into ethyl acetate. The organic layer was washed with aqueous ammonium chloride and brine and dried over sodium sulfate. The organics were removed in vacuo and the residue was filtered and washed with hexane to give 5-amino-1-(4-fluoro-phenyl)-4-(3-methoxybenzoyl)pyrazole (1.20 g).

1. customInto an oven dried flask
2. temperaturethe reaction mixture was heated
3. temperatureat reflux
4. waitthe stirring was continued for 1 h
5. customThe reaction mixture was quenched with water
6. extractionthe product was extracted into ethyl acetate
7. washThe organic layer was washed with aqueous ammonium chloride and brine
8. dry with materialdried over sodium sulfate
9. customThe organics were removed in vacuo
10. filtrationthe residue was filtered
11. washwashed with hexane