反应详情

温度

60 °C

To a suspension of 4-nitroso-2-phenyl-2H-pyrazol-3-ylamine (100 mg, 0.53 mmol) in EtOH (1 mL) is added SnCl3-2H2O (240 mg, 1.06 mmol). The mixture is then heated to 60° C. for 30 min. After cooling down the mixture, it is poured into a mixture of EtOAc (20 mL) and saturated aqueous NaHCO3 solution (20 mL). The solid is removed by filtration through Celite. The filtrate is put into separatory funnel to collect the organic layer, which is washed with brine and dried over MgSO4. After filtering off the drying agent, the filtrate is concentrated to provide the crude 2-phenyl-2H-pyrazole-3,4-diamine (˜25 mg) and used immediately for next step.

1. additionis added SnCl3-2H2O (240 mg, 1.06 mmol)
2. temperatureAfter cooling down the mixture, it
3. customThe solid is removed by filtration through Celite
4. customThe filtrate is put into separatory funnel
5. customto collect the organic layer, which
6. washis washed with brine
7. dry with materialdried over MgSO4
8. filtrationAfter filtering off the drying agent
9. concentrationthe filtrate is concentrated