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Hydrochloric Acid → 6-[N-(5-Chloro-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]-3-cyanopyridazine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Methanesulfonyl chloride | HCID 31297 | — |
| 反応物 | 6-[N-(5-Chloro-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]pyridazine-3-carboxamide | HCID 18693258 | — |
| 溶媒 | Pyridine | HCID 1049 | — |
| 生成物 | 6-[N-(5-Chloro-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]-3-cyanopyridazine | HCID 18693238 | 126.4% |
反応手順
To a solution of 6-[N-(5-chloro-2-(2-methylprop-2-en-1-yloxy)benzyl)-N-ethylamino]-pyridazine-3-carboxamide (example 18) (210 mg, 0.6 mmol) in pyridine (10 ml) at 0° C. was added methane sulfonyl chloride (0.5 ml, 0.6 mmol) and the mixture allowed to stir (gradually coming to an ambient temperature as the ice melts) for 60 hours. The solution was poured into 2 N hydrochloric acid (50 ml) over ice and the product extracted with diethyl ether (200 ml), washed with water (3×200 ml), dried over anhydrous magnesium sulphate and the solvent removed in vacuo to give the title compound as a brown gum (260 mg) which was used without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06100258 |
| 出典データセット | uspto-grants-2000_08 |
| ORD ID | ord-28fd233580a849cf9c7979c101dbe3ca |
| 出典メモ | uspto-grants-2000_08 |