関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Hydroquinone | HCID 785 | — |
| 反応物 | Sulfuric Acid | HCID 1118 | — |
| 反応物 | Azobenzene | HCID 2272 | — |
| 反応物 | Sodium Hydroxide | HCID 14798 | — |
| 反応物 | 4-Methyl-2-[2-(2-nitrophenyl)diazenyl]phenol | HCID 74029 | — |
| 反応物 | (2R,3S,4R,5R)-2,3,4,5,6-pentahydroxyhexanal | HCID 107526 | — |
| 溶媒 | Water | HCID 962 | — |
| 溶媒 | Toluene | HCID 1140 | — |
| 生成物 | 2-(2-hydroxy-5-methylphenyl)benztriazole N-oxide | HCID 13214646 | 99.2% |
反応手順
Example 5 of EP 0,257,151 is duplicated. Water (70 ml), 97% sodium hydroxide (5.2 g), 2-nitro-2'-hydroxy-5'-methylazobenzene (12.9 g) and toluene (10 ml) are mixed and heated to 60° C. After stirring, hydroquinone (0.6 g) is added, and glucose (5.0 g) is added to the mixture over one hour at 40° to 45° C. The mixture is further stirred two hours, and the azobenzene disappears. The reaction liquor is neutralized with 62% sulfuric acid (5.8 g), and is cooled to 20° C. to precipitate a crystal. The crystal thus precipitated is separated filtration to obtain a wet product 12 g of 2-(2'-hydroxy-5'-methylphenyl)benzotriazole-N-oxide (dry weight 10.8 g, yield: 90.0%, and melting point: 138° to 140° C.).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| 特許番号 | US05262541 |
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| 出典データセット | uspto-grants-1993_11 |
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| ORD ID | ord-f8ab98d1deec4391a4f841f3ff10dc4a |
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| 出典メモ | uspto-grants-1993_11 |
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