関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Tetrahydrofuran | HCID 8028 | — |
| 反応物 | Hydrazine hydrate (1:1) | HCID 24654 | — |
| 反応物 | 2-Chloro-4-cyanopyridine | HCID 568638 | — |
| 溶媒 | 1-Butanol | HCID 263 | — |
| 生成物 | 2-Hydrazinylpyridine-4-carbonitrile | HCID 20118714 | 18% |
反応手順
To a solution of 2-chloropyridine-4-carbonitrile (20.0 g, 144 mmol) in 1-butanol (150 mL) was added 1 M solution of hydrazine hydrate in THF (303 mL, 303 mmol) dropwise at rt. It was then heated at 60° C. overnight. The mixture was concentrated, and the residue was purified by flash column chromatography (CH2Cl2/MeOH=20/1) to afford the title compound (3.5 g, 18%) as a white solid. [M+H] Calc'd for C6H6N4, 135. Found, 135.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US09107916B2 |
|---|
| 出典データセット | uspto-grants-2015_08 |
|---|
| ORD ID | ord-26ee47ec087e4b198265ccbb98f6a1de |
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| 出典メモ | uspto-grants-2015_08 |
|---|
