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Aniline → 2-Aminophenyl-4-nitro-benzonitrile
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Aniline | HCID 6115 | — |
| 反応物 | N-methyl-2-pyrrolidone | HCID 13387 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 2-Chloro-4-nitrobenzonitrile | HCID 141401 | — |
| 溶媒 | Ethyl Acetate | HCID 8857 | — |
| 生成物 | 2-Aminophenyl-4-nitro-benzonitrile | HCID 17947957 | 88.4% |
反応手順
2-Chloro-4-nitro-benzonitrile (Aldrich) (3.64 g, 20 mmol), aniline (2 mL, 22 mmol), 1-methyl-2-pyrollidinone (10 mL) and diisopropylethylamine (4 mL) were combined and heated to 120° under Ar for 18 h, cooler poured into EtOAc (150 mL), washed with H20 (3×50 mL) and satd aq NaCl (50 mL), dried (Na2SO4), concentrated, and the residue was triturated with hexane, filtered and the solid was washed with hexane and dried in vacuo to afford 4.23 g (88%) of the title compound as a light green solid. 1H NMR (400) MHz, δ: 8.45 (finely split doublet, 1), 8.19 (dd, 1), 7.48 (m,3), 7.28 (d,2), 7.06 (d,1), 6.96 (br s,1).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06982270B1 |
| 出典データセット | uspto-grants-2006_01 |
| ORD ID | ord-5a79adfa8994446aaeb07317d99fe9e9 |
| 出典メモ | uspto-grants-2006_01 |