関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetylcysteamine | HCID 14484 | — |
| 反応物 | Sodium hydride | HCID 24758 | — |
| 反応物 | Imidazo(1,2-b)pyridazine, 6-chloro- | HCID 138828 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-(2-Acetylaminoethylthio)imidazo[1,2-b]pyridazine | HCID 19854507 | 77.2% |
反応手順
To 30 ml of ethanol is added 1.79 g of N-acetylcysteamine and with ice-cooling and stirring, 720 mg of sodium hydride (oily, 60 wt.%) is added. Then, 1.54 g of 6-chloroimidazo[1,2-b]pyridazine is further added and the mixture is stirred at 50° C. for 4 hours. The solvent is distilled off under reduced pressure and the residue is diluted with a saturated aqueous solution of sodium hydrogen carbonate and extracted with chloroform. The extract is dried over magnesium sulfate and the solvent is distilled off under reduced pressure. The residue is subjected to silica gel (50 g) column chromatography and after the column is washed with ethyl acetate, elution is carried out with acetone. The eluate is concentrated under reduced pressure to give 1.83 g of 6-(2-acetylaminoethylthio)imidazo[1,2-b]pyridazine as colorless powders.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04921851 |
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| 出典データセット | uspto-grants-1990_05 |
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| ORD ID | ord-e46363168c7c4e1ea3beb213db55afd9 |
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| 出典メモ | uspto-grants-1990_05 |
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