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2,5-Dimethylaniline → 2-Methylpentane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2,5-Dimethylaniline | HCID 7259 | — |
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | 2,4-Dichloropyrimidine | HCID 77531 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-Methylpentane | HCID 7892 | — |
| 生成物 | 2-Chloro-4-(2,5-dimethylanilino)pyrimidine | HCID 11310850 | — |
反応手順
2,4-Dichloropyrimidine (500 mg, 3.36 mmol), 2,5-dimethylaniline (407 mg, 3.36 mmol) and triethylamine (0.51 ml, 3.69 mmol) were dissolved in EtOH (5 ml) with stirring. The reaction mixture was heated at reflux for 12 hours, cooled and evaporated onto silica (5 ml). The residue was purified by column chromatography and eluted with EtOAc (30%): isohexane to give the title product as a waxy solid on evaporation (514 mg, 66%). NMR (300 MHz): 2.1 (s, 3H), 2.27 (s, 3H), 6.42 (d. 1H), 6.99 (d, 1H), 7.08 (s, 1H). 7.18 (d, 1H), 8.03 (d, 1H), 9.45 (s, 1H); m/z: (ES+) 234.3 (MH+).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07176212B2 |
| 出典データセット | uspto-grants-2007_02 |
| ORD ID | ord-36c0c7568fde4d02bed8f71c2b1944d0 |
| 出典メモ | uspto-grants-2007_02 |