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Nitrogen → 2-Acetamido-5-aminopyridine
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Nitrogen | HCID 947 | — |
| 反応物 | 2-Acetamido-5-nitropyridine | HCID 345125 | — |
| 反応物 | Ammonium formate | HCID 2723923 | — |
| 触媒 | Palladium | HCID 23938 | — |
| 溶媒 | Methanol | HCID 887 | — |
| 溶媒 | Dimethylformamide | HCID 6228 | — |
| 生成物 | 2-Acetamido-5-aminopyridine | HCID 2735219 | 88.2% |
反応手順
A N2 covered solution of 1.19 g (6.6 mmol) of the product from Step 1 in 24 ml of DMF was treated with 2.07 g (32.9 mmol) of ammonium formate followed by 0.36 g of palladium on carbon catalyst. After stirring vigorously at room temperature for 17 hours, the reaction was diluted with MeOH and the catalyst was removed by filtration through celite. The filtrate was concentrated in vacuo and the residue was chromatographed over silica gel (3% MeOH: 0.3% NH4OH: CH2Cl2) to yield 0.876 g, m.p. 152°-153.5° C. (88.2%) of the titled product.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US05567722 |
| 出典データセット | uspto-grants-1996_10 |
| ORD ID | ord-96c5e8a930fb438ebc8d061ffae6a959 |
| 出典メモ | uspto-grants-1996_10 |