関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Sodium Iodide | HCID 5238 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | 6-Chloropyridazin-3-ol | HCID 252828 | — |
| 反応物 | N,N-Dimethylaminoethyl chloride hydrochloride | HCID 11636816 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 6-Chloro-2-(2-(dimethylamino)ethyl)pyridazin-3(2H)-one | HCID 69306583 | 22.5% |
反応手順
To a solution of 6-chloro-2H-pyridazin-3-one (500 mg, 3.83 mmol) in 5 mL dimethylformamide was added 2-dimethylaminoethyl chloride hydrochloride (828 mg, 5.75 mmol), potassium carbonate (1.59 g, 11.5 mmol) and sodium iodide (632 mg, 4.21 mmol). The mixture was stirred over night at 65° C. Solvent was evaporated. The crude product was dissolved in water and purified by preparative HPLC using a gradient of acetonitrile/5% acetonitrile—water phase containing 0.1 M ammonium acetate, to give 174 mg of 6-chloro-2-(2-dimethylamino-ethyl)-2H-pyridazin-3-one as light brown crystals after freeze drying (22% yield).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US07419979B2 |
|---|
| 出典データセット | uspto-grants-2008_09 |
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| ORD ID | ord-f9aa938a188a4e96a702ce5c78b1c47e |
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| 出典メモ | uspto-grants-2008_09 |
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