反应详情

A mixture of 5-amino-1-(4-fluorophenyl)-4-(3-nitrobenzoyl)pyrazole (4.0 g, 24.52), Fe powder (3.84 g, 68 mmol) and ammonium chloride (3.84, 71.78 mmol) in ethanol (135 ml) and water (64 ml) was heated at reflux under nitrogen atmosphere. After 1 h, the reaction mixture was cooled to room temperature and stirred overnight. The reaction mixture was filtered through Celite® and the filtrate was concentrated in vacuo. The residue was partitioned between water and ethyl acetate. The organic layer was separated and washed with brine, dried over sodium sulfate and concentrated in vacuo to give 5-amino-4-(3-aminobenzoyl)-1-(4-fluorophenyl)pyrazole (3.5 g) as a solid.

1. temperaturewas heated
2. temperatureat reflux under nitrogen atmosphere
3. filtrationThe reaction mixture was filtered through Celite®
4. concentrationthe filtrate was concentrated in vacuo
5. customThe residue was partitioned between water and ethyl acetate
6. customThe organic layer was separated
7. washwashed with brine
8. dry with materialdried over sodium sulfate
9. concentrationconcentrated in vacuo