関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Potassium Hydroxide | HCID 14797 | — |
| 反応物 | 4-Bromo-N1-methylbenzene-1,2-diamine | HCID 11298593 | — |
| 反応物 | Sodium Nitrite | HCID 23668193 | — |
| 溶媒 | Hydrochloric Acid | HCID 313 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 5-bromo-1-methyl-1H-1,2,3-benzotriazole | HCID 57642578 | 33.7% |
反応手順
To a solution of 4-bromo-N1-methylbenzene-1,2-diamine (4.2 g, 21 mmol) in hydrochloric acid (2N, 50 ml) was added a solution of NaNO2 (1.52 g, 22 mmol) in water (5 ml) at 0° C. The resulting solution was stirred for 4 h at 0-10° C., adjusted to pH 8 with potassium hydroxide (3N), extracted with dichloromethane (2×200 ml), and the organic layers combined and concentrated under vacuum to give a residue, which was purified via silica gel chromatography (50% dichloromethane in petroleum ether) to afford 5-bromo-1-methyl-1H-benzo[d][1,2,3]triazole as a red solid (1.5 g, 31%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08912188B2 |
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| 出典データセット | uspto-grants-2014_12 |
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| ORD ID | ord-10bbfb56008b4553ae3bb244b82cbebf |
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| 出典メモ | uspto-grants-2014_12 |
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