関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Ammonium formate | HCID 2723923 | — |
| 反応物 | Chloro-4-(4-(2-nitroethyl)phenoxy)-2-(trifluoromethyl)benzene | HCID 67775633 | — |
| 触媒 | Zinc | HCID 23994 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(4-(4-Chloro-3-(trifluoromethyl)phenoxy)phenyl)ethanamine | HCID 67775548 | 36.5% |
反応手順
To a solution of 1-chloro-4-(4-(2-nitroethyl)phenoxy)-2-(trifluoromethyl)benzene (21 g, 60.7 mmol) and ammonium formate (30.6 g, 486 mmol) in methanol (250 mL) and water (250 mL), was added zinc powder (15.89 g, 243 mmol). The reaction mixture was stirred at 80° C. for 2 h, filtered through a glass grit and washed with methanol. The filtrate was concentrated and the residue was extracted with DCM (200 mL), and then washed with sat. NaHCO3 (100 mL), brine, and dried over anhydrous Na2SO4 and concentrated. Purification via FC (DCM/CH3OH=100/8) afforded the title compound (7.0 g) as a yellow oil.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US09273054B2 |
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| 出典データセット | uspto-grants-2016_03 |
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| ORD ID | ord-66714892334d4d1e838afa23e3f840d3 |
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| 出典メモ | uspto-grants-2016_03 |
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