反应详情

温度

60 °C

A suspension of nickel boride (3.56 g) and 1N HCl (16 mL) in methanol (65 mL) was added to ethyl 3-phenyl-4-(4-chloro-2-nitrobenzoyl)-1H-pyrazole-5-carboxylate (1.5 g, 3.7 mmol) and the mixture heated to 60° C. for 18 hours. The reaction mixture was filtered and the filtrate concentrated via rotovap to a green solid (2.38 g). The solid was dissolved in ethyl acetate (100 mL) and extracted with water (2×50 mL) and brine (1×50 mL). The organic layer was dried over sodium sulfate and concentrated to a dark green oil (1.5 g) which was washed with a small amount of hexanes to yield the title compound as a yellow solid (0.855 g, 62%).

1. filtrationThe reaction mixture was filtered
2. concentrationthe filtrate concentrated via rotovap to a green solid (2.38 g)
3. dissolutionThe solid was dissolved in ethyl acetate (100 mL)
4. extractionextracted with water (2×50 mL) and brine (1×50 mL)
5. dry with materialThe organic layer was dried over sodium sulfate
6. concentrationconcentrated to a dark green oil (1.5 g) which
7. washwas washed with a small amount of hexanes