関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 3-Chloropropane-1-sulfonamide | HCID 13614818 | — |
| 反応物 | 3,6-Dichloroimidazo[1,2-b]pyridazine | HCID 15271014 | — |
| 反応物 | Sodium methanolate methanol | HCID 23694274 | — |
| 反応物 | Potassium hydrogensulfide ethanol | HCID 86746192 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 生成物 | 3-Chloro-6[(3-sulfamoylpropyl)thio]imidazo[1,2-b]pyridazine | HCID 10447903 | — |
反応手順
To a solution of 1.57 g of 3-chloro-1-propanesulfonamide in 20 ml of methanol was added 20ml of 2N-potassium hydrogensulfide-ethanol solution, followed by heating at 70° C. for 50 minutes. Then, 1.48 g of 28% sodium methoxide-methanol solution and 1.32g of 3,6-dichloroimidazo[1,2-b]pyridazine were added to the reaction mixture and refluxed at 100° C. for 3 hours. The mixture was concentrated under reduced pressure, and to the residue was added 20 ml of water, which was adjusted to pH 7.0 with 1N-hydrochloric acid. The precipitated crystals were collected by filtration and recrystallized from methanol and ethyl ether to obtain 1.12 g of the title compound.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05155108 |
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| 出典データセット | uspto-grants-1992_10 |
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| ORD ID | ord-5d531bf8726249378baa5fe29c51d349 |
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| 出典メモ | uspto-grants-1992_10 |
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