関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1-Butanol | HCID 263 | — |
| 反応物 | Potassium Carbonate | HCID 11430 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 2-Chloro-3-methoxypyridine | HCID 104252 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-Hydrazinyl-3-methoxypyridine | HCID 18545404 | — |
反応手順
To 50 ml of a butanol solution of 9.376 g of 2-chloro-3-methoxypyridine were added 16 ml of hydrazine monohydrate and 9.03 g of anhydrous potassium carbonate, and the mixture was heated under reflux for 20 hours. After cooling, the reaction mixture was poured into 200 ml of water and extracted with a mixed solvent of methanol-chloroform (1:9 by volume). The organic layer was washed with a saturated sodium chloride aqueous solution, and dried over anhydrous sodium sulfate. The solvent was removed by evaporation. The residue was subjected to silica gel column chromatography using a mixture of chloroform-methanol (20:1 by volume) as an eluate. The fraction containing the desired compound was concentrated to afford 5.952 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 | US06169086A |
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| 出典データセット | uspto-grants-2001_01 |
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| ORD ID | ord-2904f9b1bac34986b09014d2022e536f |
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| 出典メモ | uspto-grants-2001_01 |
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