関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ethyl Acetate | HCID 8857 | — |
| 反応物 | Sodium Bicarbonate | HCID 516892 | — |
| 反応物 | 5-Amino-4-nitroso-1-phenylpyrazole | HCID 10750106 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-phenyl-2H-pyrazole-3,4-diamine | HCID 10654819 | 27.1% |
反応手順
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.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08158634B2 |
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| 出典データセット | uspto-grants-2012_04 |
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| ORD ID | ord-d81e0ae429fe4de896cd1a5f10364049 |
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| 出典メモ | uspto-grants-2012_04 |
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