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N-[4-bromo-3-(trifluoromethyl)phenyl]-2-nitrobenzamide → 2-Amino-N-(4-bromo-3-trifluoromethylphenyl)benzamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | N-[4-bromo-3-(trifluoromethyl)phenyl]-2-nitrobenzamide | HCID 1300995 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 2-Amino-N-(4-bromo-3-trifluoromethylphenyl)benzamide | HCID 11268358 | — |
反応手順
A solution of 2-nitro-N-(4-bromo-3-trifluoromethylphenyl)benzamide (intermediate 1a; 32 g, 82 mmol) in methanol (1000 mL) is hydrogenated at atmospheric pressure over Raney nickel (6 g) at 21° C. The calculated amount of hydrogen is taken up after 7 hours. The mixture is filtered and the solvent is evaporated under reduced pressure to yield the crude product which is purified by recrystallisation from diethylether-hexane to give the title compound as a colourless crystalline solid, m.p. 142–144° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07067543B2 |
| 出典データセット | uspto-grants-2006_06 |
| ORD ID | ord-707fcf78eb4a4d9c8e1d8c4fb932019d |
| 出典メモ | uspto-grants-2006_06 |