関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 1,2-Dichlorobenzene | HCID 7239 | — |
| 反応物 | Chloric acid | HCID 19654 | — |
| 反応物 | 2-(6-Acetoxy-2-naphthoylamino)-4-butylphenol | HCID 19795411 | — |
| 溶媒 | Water | HCID 962 | — |
| 生成物 | 2-(6-Hydroxy-2-naphthyl)-5-butylbenzooxazole | HCID 135727113 | 48% |
反応手順
5.40 g (14.3 m mole) of 2-(6-acetoxy-2-naphthoylamino)-4-butylphenol, 0.43 g of p-toluenesulfuric acid monohydrate and 40 ml of O-dichlorobenzene were placed in a 100 ml round-bottom flask, followed by heating and stirring for 30 minutes at 200-203° C. After the reaction, O-dichlorobenzene was distilled off under reduced pressure. To the resultant, 2.00 g (30.3 m mole) of potassium hydroxide and 60 ml of ethanol were added, followed by heating and stirring for 20 minutes at 60° C. After the reaction, the reaction mixture was poured into 600 ml of water. To the reaction mixture, 8 ml of chloric acid was added to precipitate a crystal. The crystal was filtered, washed with water and recrystallized from a mixture solvent of acetoneethanol to obtain 2.18 g of 2-(6-hydroxy-2-naphthyl)-5-butylbenzooxazole (Yield: 42.4%).
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US05244596 |
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| 出典データセット | uspto-grants-1993_09 |
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| ORD ID | ord-f954faeda5054c7c942ac3ce9dae5608 |
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| 出典メモ | uspto-grants-1993_09 |
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