反应详情

温度

70 °C

To a mixture of 980 mg of 5-(4-bromo-2-nitrophenyl)-1-cyclopentyl-1H-pyrazole, 9.8 mL of tetrahydrofuran, 19.6 mL of ethanol, and 2.9 mL of water was added 102 mg of ammonium chloride, followed by heating at 70° C. 1.03 g of reduced iron was added thereto, followed by heating to reflux for 4 hours, and cooling to room temperature. The insoluble material was filtered through celite, the filtrate was concentrated, and a mixture of chloroform/water was added thereto. The aqueous layer was separated, and then the organic layer was washed with saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure and the residue was purified by silica gel column chromatography (n-hexane/ethyl acetate) to obtain 815 mg of 5-bromo-2-(1-cyclopentyl-1H-pyrazol-5-yl)aniline.

1. temperatureby heating
2. temperatureto reflux for 4 hours
3. temperaturecooling to room temperature
4. filtrationThe insoluble material was filtered through celite
5. concentrationthe filtrate was concentrated
6. additiona mixture of chloroform/water
7. additionwas added
8. customThe aqueous layer was separated
9. washthe organic layer was washed with saturated brine
10. dry with materialdried over anhydrous magnesium sulfate
11. customThe solvent was evaporated under reduced pressure
12. customthe residue was purified by silica gel column chromatography (n-hexane/ethyl acetate)