関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 2-Amino-3-nitro-6-(3-trifluoromethyl-piperidin-1-yl)benzonitrile | HCID 67957975 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2,3-Diamino-6-(3-trifluoromethyl-piperidin-1-yl)benzonitrile | HCID 67958270 | — |
反応手順
A mixture of 2-amino-3-nitro-6-(3-trifluoromethyl-piperidin-1-yl)benzonitrile (200 mg, 0.64 mmol), Fe (178 mg, 3.18 mmol), aqueous NH4Cl (5 mL) and EtOH (5 mL) was heated under Ar at 90° C. for 2 h. The mixture was thereafter basicified to pH ˜9-10 and filtered through celite and the celite pad was washed with EtOH and EtOAc. The organic layer was concentrated and the residue was extracted with EtOAc. The organic layer was dried over Na2SO4, filtered and concentrated. The residue was washed with Et2O to give the sub-title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08466186B2 |
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| 出典データセット | uspto-grants-2013_06 |
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| ORD ID | ord-c6eaeed1973b47e6b1cb5934f0cd162f |
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| 出典メモ | uspto-grants-2013_06 |
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