関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Water | HCID 962 | — |
| 反応物 | Isopropyl iodide | HCID 6362 | — |
| 反応物 | Diisopropylethylamine | HCID 81531 | — |
| 反応物 | 6-Chloro-[1,2,4]triazolo[1,5-b]pyridazine-2-carboxylic acid | HCID 22989292 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | Isopropyl 6-chloro[1,2,4]triazolo[1,5-b]pyridazine-2-carboxylate | HCID 22989245 | — |
反応手順
2.14 g of 6-chloro[1,2,4]triazolo[1,5-b]pyridazine-2-carboxylic acid and 5.57 ml of N-ethyldiisopropylamine were dissolved in 30 ml of N,N-dimethylformamide; 3.23 ml of isopropyl iodide was added, followed by stirring at room temperature for 10 hours and at 50° C. for 3 hours. After cooling, water was added, followed by extraction with ethyl acetate; the extract was washed with saturated saline, dried over magnesium sulfate and concentrated under reduced pressure. The residue was subjected to silica gel column chromatography and eluted with ethyl acetate. The desired fraction was collected and concentrated under reduced pressure to yield 2.21 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 | US06627630B1 |
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| 出典データセット | uspto-grants-2003_09 |
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| ORD ID | ord-131f586a4f3c49bda5e03417908d6d78 |
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| 出典メモ | uspto-grants-2003_09 |
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