Beteiligte Stoffe
| Rolle | Name | HCID | Einwaage |
|---|
| Edukt | Ethyl Acetate | HCID 8857 | — |
| Edukt | Sodium Bicarbonate | HCID 516892 | — |
| Edukt | 5-Amino-4-nitroso-1-phenylpyrazole | HCID 10750106 | — |
| Lösungsmittel | Ethanol | HCID 702 | — |
| Produkt | 2-phenyl-2H-pyrazole-3,4-diamine | HCID 10654819 | 27,1% |
Reaktionsschritte
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.
Herkunft & Nachweise
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| Patentnummer | US08158634B2 |
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| Quelldatensatz | uspto-grants-2012_04 |
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| ORD ID | ord-d81e0ae429fe4de896cd1a5f10364049 |
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| Quellennotiz | uspto-grants-2012_04 |
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