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But-2-yn-1-amine → HCID 178449099、化合物
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | But-2-yn-1-amine | HCID 12599998 | — |
| 反応物 | HCID 178503826 | HCID 178503826 | — |
| 溶媒 | Acetonitrile | HCID 6342 | — |
| 生成物 | HCID 178449099 | HCID 178449099 | 80% |
反応手順
A mixture of 1-nitro-2-methylthio-2-{2-[(4-methyl-1H-imidazol-5-yl)methylthio]ethylamino}ethylene (2.25 g, 7.8 mmole) and 2-butyn-1-amine (2.16 g, 31.2 mmole) in acetonitrile (35 ml) was stirred under a positive pressure of nitrogen at reflux temperature for 7 hours and at room temperature for 15 hours. The solvent was removed by evaporation under reduced pressure, and the residue placed on silica gel and chromatographed by gradient elution using methylene chloride-methanol. The appropriate fractions yielded 1.93 g (80%) of the title product from acetonitrile. Recrystallization from isopropyl alcohol gave the product with mp 147.5°-151°.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US04221737 |
| 出典データセット | uspto-grants-1980_09 |
| ORD ID | ord-cb5192f8f86244b28cb277a0844b27e9 |
| 出典メモ | uspto-grants-1980_09 |