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Methyl iodide → 4-Bromo-6-chloro-2-methyl-2,3-dihydropyridazin-3-one
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Methyl iodide | HCID 6328 | — |
| 反応物 | Cesium carbonate | HCID 10796 | — |
| 反応物 | 4-Bromo-6-chloro-2,3-dihydropyridazin-3-one | HCID 11586522 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 4-Bromo-6-chloro-2-methyl-2,3-dihydropyridazin-3-one | HCID 59216474 | 97.5% |
反応手順
4-Bromo-6-chloro-2H-pyridazin-3-one (5.02 g, 23.97 mmol) was dissolved in 40 ml dimethylformamide. Cesium carbonate (9.37 g, 28.76 mmol) was added. After 5 min, iodomethane (5.103 g, 35.95 mmol) was added dropwise over 20 min. The reaction mixture was stirred 3 hours at room temperature. The precipitate was filtered off and concentrated and the resulting residue was treated with 20 ml dichloromethane. The insoluble material was filtered off again and washed with dichloromethane. The filtrate was concentrated in vacuo to yield 4-Bromo-6-chloro-2-methyl-2H-pyridazine-3-one (5.223 g, 23.37 mmol). MS (ESI) 224.9 (M+H)+
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08822457B2 |
| 出典データセット | uspto-grants-2014_09 |
| ORD ID | ord-4716460160e64d4f9fd22f14877dfffc |
| 出典メモ | uspto-grants-2014_09 |