反应详情

温度

80 °C

A solution of 5.2 g (0.013 mole) 5-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-4-fluoro-N-methyl-2-nitro-N-propylbenzenamine in 100 mL acetic acid was heated to 80° C. under a nitrogen atmosphere. The heat and nitrogen were removed and 2.2 g (0.039) mole iron powder was added in 3 portions over 5 min. The solution was stirred at 80° C. for an additional 30 min. The solution was cooled and filtered through Celite®. The filtrate was diluted with 100 mL water and extracted three times with ethyl acetate. The ethyl acetate extracts were washed with a saturated NaHCO3 solution, dried over anhydrous MgSO4, and concentrated in vacuo. The residue was purified chromatographically using 30% ethyl acetate in hexane as the eluent to give 3.85 g (80%) of 5-(4-chloro-1-methyl-5-(trifluoromethyl)-1H-pyrazol-3-yl)-4-fluoro-N-methyl-N-propyl-1, 2-benzenediamine as a light yellow oil, nD25 1.5352.

1. temperatureThe heat
2. customnitrogen were removed
3. addition2.2 g (0.039) mole iron powder was added in 3 portions over 5 min
4. temperatureThe solution was cooled
5. filtrationfiltered through Celite®
6. additionThe filtrate was diluted with 100 mL water
7. extractionextracted three times with ethyl acetate
8. washThe ethyl acetate extracts were washed with a saturated NaHCO3 solution
9. dry with materialdried over anhydrous MgSO4
10. concentrationconcentrated in vacuo
11. customThe residue was purified chromatographically