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Nitrogen mustard hydrochloride → 3-Bromo-8-(4-methyl-piperazin-1-yl)-quinoline
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen mustard hydrochloride | HCID 5935 | — |
| 反応物 | Sodium Carbonate | HCID 10340 | — |
| 反応物 | 3-Bromoquinolin-8-amine | HCID 15112545 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 3-Bromo-8-(4-methyl-piperazin-1-yl)-quinoline | HCID 67313624 | 49% |
反応手順
bis-(2-Chloro-ethyl)-methyl-amine hydrochloride (3.7 g, 19.2 mmol) and sodium carbonate (9.0 g, 85 mmol) were added to a suspension of 3-bromo-quinolin-8-ylamine (3.9 g, 17.5 mmol) (for synthesis see Gershon et al., Monatsh. Chem., 1991, 122, 935) in n-butanol (70 ml). The stirred suspension was heated at reflux for 72 h. The reaction mixture was cooled to ambient temperature, diluted with dichloromethane (300 ml) and the solution washed with water (300 ml), dried (MgSO4) and concentrated in vacuo to an oil. The oil was purified by chromatography over silica gel eluting with a gradient of methanol/dichloromethane to afford the title compound (D1) as an oil (2.6 g, 8.5 mmol, 49%);
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US07452888B2 |
| 出典データセット | uspto-grants-2008_11 |
| ORD ID | ord-4a128299e4d74e9bad1f5963b56a11e9 |
| 出典メモ | uspto-grants-2008_11 |