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Hydrazine hydrate (1:1) → 5-Amino-2-(3-aminopropyl)-3-methylpyridine
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 | 5-Nitro-2-(2-cyanoethyl)-3-methylpyridine | HCID 19851777 | — |
| 触媒 | Nickel | HCID 935 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 5-Amino-2-(3-aminopropyl)-3-methylpyridine | HCID 19851780 | 145.2% |
反応手順
Raney nickel (24 g) was added to a stirred solution under nitrogen of 5-nitro-2-(2-cyanoethyl)-3-methylpyridine (10.36 g) in ethanol (700 ml). Hydrazine hydrate (13.5 ml) in ethanol (30 ml) was added over 2.75 hr., followed by further additions of Raney nickel (15 g) and hydrazine hydrate (60 ml) over two days which included two periods of eight hours at 50° C. The solution was decanted off, filtered through a hyflo pad and concentrated to dryness to give a green oil (13 g). This oil was chromatographed on silica in ethylacetate/ethanol/0.880 ammonia 15:10:2 to give the title compound as an oil (8.14 g).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04764519 |
| 出典データセット | uspto-grants-1988_08 |
| ORD ID | ord-e65b65387f754e1a8c83ddf37853aff1 |
| 出典メモ | uspto-grants-1988_08 |