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Hydrazine hydrate (1:1) → 6-cyclopropyl-N-(6-(hydrazinecarbonyl)pyridin-2-yl)-3,4'-bipyridine-2'-carboxamide
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | Methyl 6-(6-cyclopropyl-3,4'-bipyridine-2'-carboxamido)picolinate | HCID 66848750 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 6-cyclopropyl-N-(6-(hydrazinecarbonyl)pyridin-2-yl)-3,4'-bipyridine-2'-carboxamide | HCID 58103016 | 47% |
反応手順
The methyl 6-(6-cyclopropyl-3,4′-bipyridine-2′-carboxamido)picolinate from the previous step were suspended in ethanol (20 mL), hydrazine hydrate (700 μL, 14.4 mmol) was added, and the reaction was heated to reflux for 4 hours. The reaction mixture was concentrated and the resultant solids were suspended in acetronitrile and collected by filtration. The solids were washed with acetonitrile (2×100 mL) and diethyl ether (2×100 mL), and dried under reduced pressure to afford 1.21 g (47% yield) of 6-cyclopropyl-N-(6-(hydrazinecarbonyl)pyridin-2-yl)-3,4′-bipyridine-2′-carboxamide as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US08598360B2 |
| 出典データセット | uspto-grants-2013_12 |
| ORD ID | ord-a3dd9275771a40dab782e3d9303c0021 |
| 出典メモ | uspto-grants-2013_12 |