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Hydrazine hydrate (1:1) → 4-chloro-N-(6-(hydrazinecarbonyl)pyridin-2-yl)picolinamide
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 | 6-[(4-Chloro-pyridine-2-carbonyl)-amino]-pyridine-2-carboxylic acid methyl ester | HCID 66848725 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 4-chloro-N-(6-(hydrazinecarbonyl)pyridin-2-yl)picolinamide | HCID 58103019 | 92% |
反応手順
The crude 6-[(4-chloro-pyridine-2-carbonyl)-amino]-pyridine-2-carboxylic acid methyl ester from the previous step (25.3 g, 87.8 mmol) was suspended in ethanol (200 mL), and hydrazine hydrate (21.3 mL, 439 mmol) was added. The reaction mixture was refluxed for 4 hours, solvent removed under reduced pressure, and the residue suspended in acetonitrile and collected by filtration. The solids were washed with acetonitrile (2×100 mL) and diethylether (2×100 mL), and dried under reduced pressure to afford 25.3 g (92% yield) of 4-chloro-N-(6-(hydrazinecarbonyl)pyridin-2-yl)picolinamide as a white solid.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US09067933B2 |
| 出典データセット | uspto-grants-2015_06 |
| ORD ID | ord-c21df8faeca9485cbb56c4076a2721da |
| 出典メモ | uspto-grants-2015_06 |