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Triethylamine → 1-(2-Hex-5-ynoylperhydropyridazinyl)-3,3-dimethylpentane-1,2-dione
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | Triethylamine | HCID 8471 | — |
| 反応物 | Isobutyl chloroformate | HCID 62365 | — |
| 反応物 | 5-Hexynoic acid | HCID 143036 | — |
| 反応物 | 3,3-Dimethyl-1-perhydropyridazinylpentane-1,2-dione | HCID 69417804 | — |
| 溶媒 | Dichloromethane | HCID 6344 | — |
| 生成物 | 1-(2-Hex-5-ynoylperhydropyridazinyl)-3,3-dimethylpentane-1,2-dione | HCID 18470065 | 63% |
反応手順
To a solution of 5-hexynoic acid (0.467 g, 4 mmol) in 10 ml CH2Cl2 was added triethylamine (0.56 ml, 4 mmol), followed by isobutyl chloroformate (0.53 ml, 4 mmol) at 0° C. After stirring for 5 minutes, a solution of 3,3-dimethyl-1-perhydropyridazinyl pentane-1,2-dione (0.424 g, 2 mmol) in 1 ml CH2Cl2 was added. The reaction was gradually warmed up to room temperature. The crude material was subject to silica gel purification to yield final product as clear oil (0.385 g, 63%). 1H NMR (CDCl3, 400 MHz) δ 0.91 (t, 3H, J=7.0); 1.26 (s, 6H); 1.76(m, 8H); 2.28 (m, 2H); 2.50 (m, 2H); 2.88 (m, 2H); 3.60 (m, 1H); 4.50 (m, 2H).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06417189B1 |
| 出典データセット | uspto-grants-2002_07 |
| ORD ID | ord-cff6e2b7d0f34adfafed6d40de6e5289 |
| 出典メモ | uspto-grants-2002_07 |