関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | 6-Bromo-2-(methylthio)benzoxazole | HCID 13314821 | — |
| 反応物 | 4-(N-methylamino)phenol acetate | HCID 20826194 | — |
| 溶媒 | Acetic Acid | HCID 176 | — |
| 生成物 | 4-[N-Methyl-N-(6-bromo-2-benzoxazolyl)amino]phenol | HCID 13314820 | 43.9% |
反応手順
An intimate mixture of 4-(N-methylamino)phenol acetate (7.3 g, 0.04 mole) and 6-bromo-2-(methylthio)benzoxazole (6.0 g, 0.025 mole) was prepared and heated on an oil bath to a temperature of 180° C. The mixture was heated at this temperature for a period of 4 hours during which time acetic acid distilled from the mixture and methyl mercaptan was evolved and was trapped in aqueous sodium hydroxide. The mixture was cooled to form a solid and the solid was extracted with hot toluene (4×100 ml). The toluene solution was filtered hot and the solvent removed by distillation to give a brown solid. The solid was recrystallised from toluene to give the title compound as a grey solid (3.5 g), mp 195° C.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US04314065 |
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| 出典データセット | uspto-grants-1982_02 |
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| ORD ID | ord-2e2ca9a1260e4f188f9a734d27c27aa9 |
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| 出典メモ | uspto-grants-1982_02 |
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