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Hydrochloric Acid → 3-Chloro-3-methyl-2-nitroso-1-(5-methyl-2-nitro-1H-imidazol-1-yl)butane
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | Isoamyl nitrate | HCID 10985 | — |
| 反応物 | 1-(5-methyl-2-nitro-1H-imidazol-1-yl)-3-methyl-2-butene | HCID 15186015 | — |
| 生成物 | 3-Chloro-3-methyl-2-nitroso-1-(5-methyl-2-nitro-1H-imidazol-1-yl)butane | HCID 15186017 | 60% |
反応手順
3-Chloro-3-methyl-2-nitroso-1-(5-methyl-2-nitro-1H-imidazol-1-yl) butane was prepared in 60% yield from 1-(5-methyl-2-nitro-1H-imidazol-1-yl)-3-methyl-2-butene (1.0 g, 5.12 mmol, Example 27), isoamyl nitrate (5.0 mL) and concentrated HCl (5.0 mL) following the procedure described for the preparation of its positional isomer (Example 27B) as a light blue solid; mp. 102-105° C. (decomp); 1H NMR (DMSO-d6) δ 1.73 [s, 6H, C(CH3)2], 2.32(s, 3H, imi-CH3), 5.53(s, 2H, NCH2), 6.97 ( s. 1H, imi-CH) and 11.58 (s, 1H, NOH). MS m/e 261 (M+H)+.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06359120B1 |
| 出典データセット | uspto-grants-2002_03 |
| ORD ID | ord-d4c52a84c0cd49e38b76c22e563f7c75 |
| 出典メモ | uspto-grants-2002_03 |