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Formic Acid → 2,4-Diaminonicotinaldehyde
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Formic Acid | HCID 284 | — |
| 反応物 | 4,6-Diaminonicotinonitrile | HCID 295896 | — |
| 反応物 | HCID 178418361 | HCID 178418361 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2,4-Diaminonicotinaldehyde | HCID 21850029 | — |
反応手順
A suspension of 13.4 g of 2,4-diamino-5-cyanopyridine from Example 14, 2 g of Raney nickel catalyst, 40 mL of 97-100% formic acid, and 80 mL of water were shaken in a Parr apparatus under an atmosphere of nitrogen until the requisite amount of hydrogen was consumed. The solvents were removed under reduced pressure and the residue treated with 17 mL of concentrate HCl. The resulting pink solid was slurried in a small amount of water, filtered, washed with isopropyl alcohol, followed by diethylether, and dried. Crystallization from ethanol afforded 6.5 g of the title compound 2,4-diaminonicotinaldehyde.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05733913 |
| 出典データセット | uspto-grants-1998_03 |
| ORD ID | ord-66fceab868444128830a463ef7b06941 |
| 出典メモ | uspto-grants-1998_03 |