関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | Ammonium Chloride | HCID 25517 | — |
| 反応物 | 1-[4-(2-Methyl-[1,3]dioxolan-2-yl)-butyl]-3-nitro-1H-pyrazole | HCID 66928335 | — |
| 触媒 | Iron | HCID 23925 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 1-[4-(2-Methyl-[1,3]dioxolan-2-yl)-butyl]-1H-pyrazol-3-ylamine | HCID 66928481 | — |
反応手順
In a flame dried round-bottomed flask equipped with a magnetic stir bar and under inert atmosphere (N2), a mixture of 1-[4-(2-methyl-[1,3]dioxolan-2-yl)-butyl]-3-nitro-1H-pyrazole (300 mg, 1.18 mmol), iron powder (199 mg, 3.53 mmol) and NH4Cl (317 mg, 5.88 mmol) in a mixture of EtOH (4.0 mL) and water (2.0 mL) was stirred at 75° C. for 30 min. The reaction mixture was filtered while hot and concentrated under reduced pressure. CH2Cl2 (20 mL) was added followed by water (20 mL). The aq. layer was extracted with CH2Cl2 (3×10 mL) and the combined org. extracts were dried over MgSO4, filtered, and the solvents were removed under reduced pressure to give the title compound as a colorless oil. LC-MS-conditions 02: tR=0.59 min; [M+H]+=226.47.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08288419B2 |
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| 出典データセット | uspto-grants-2012_10 |
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| ORD ID | ord-6fb3ff596a6e4d399eec2534a04669eb |
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| 出典メモ | uspto-grants-2012_10 |
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