関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 3-cyclopropyl-1-((6-methylpyridin-2-yl)methyl)-4-nitro-1H-indazole | HCID 67260809 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Water ethanol | HCID 19096565 | — |
| 生成物 | 3-cyclopropyl-1-((6-methylpyridin-2-yl)methyl)-1H-indazole-4-amine | HCID 67259272 | 84.9% |
反応手順
To a suspension of 3-cyclopropyl-1-((6-methylpyridin-2-yl)methyl)-4-nitro-1H-indazole (22.01 g, 71.38 mmol) in EtOH/H2O (200 mL/50 mL) was added iron powder (79.73 g, 1428 mmol) and NH4Cl (3.818 g, 71.38 mmol). The reaction mixture was heated to reflux for three hours, cooled to 60° C. and filtered through a pad of Celite. The pad of Celite was washed with 20:1 EtOH/Et3N (800 mL) and 1:1 MeOH/DCM (600 mL). The combined filtrate was concentrated under reduced pressure. The residue was dissolved in EtOAc (800 mL), washed with saturated NaHCO3 aqueous solution, dried (Na2SO4) and concentrated under reduced pressure to give the product (16.87 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08841455B2 |
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| 出典データセット | uspto-grants-2014_09 |
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| ORD ID | ord-23a6bef378da49d3a527ffbf1fd547a2 |
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| 出典メモ | uspto-grants-2014_09 |
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