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2-Hydrazinobenzoic acid → 2-(3,5-bis(2-hydroxyphenyl)-1H-1,2,4-triazol-1-yl)benzoic acid
関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|---|---|---|
| 反応物 | 2-Hydrazinobenzoic acid | HCID 79223 | — |
| 反応物 | 2-(2-Hydroxyphenyl)-4H-1,3-benzoxazin-4-one | HCID 135685723 | — |
| 溶媒 | Ethanol | HCID 702 | — |
| 生成物 | 2-(3,5-bis(2-hydroxyphenyl)-1H-1,2,4-triazol-1-yl)benzoic acid | HCID 135817473 | — |
反応手順
4.8 g of 2-(2-hydroxyphenyl)benz[e][1,3]oxazin-4-one and 3.5 g of 2-hydrazinobenzoic acid are boiled under reflux for 4 h in 10 ml of ethanol. The mixture is cooled, poured onto water and extracted with ethyl acetate. The combined organic phases are dried over sodium sulfate and concentrated on a rotary evaporator. The residue is crystallized from ethyl acetate/hexane. After drying, 2-[3,5-bis(2-hydroxyphenyl)-[1,2,4]triazol-1-yl]benzoic acid is obtained as colorless crystals of m.p. 132-138° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| 特許番号 | US06596750B2 |
| 出典データセット | uspto-grants-2003_07 |
| ORD ID | ord-bb5d675b5a0c42ba9b3d7494eb5997eb |
| 出典メモ | uspto-grants-2003_07 |