関与物質
| 役割 | 名称 | HCID | 仕込み量 |
|---|
| 反応物 | Acetic Acid | HCID 176 | — |
| 反応物 | Hydrochloric Acid | HCID 313 | — |
| 反応物 | 4-Chlorobenzaldehyde | HCID 7726 | — |
| 反応物 | 2,3-Pentanedione, 2-oxime | HCID 6797453 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(4-Chlorophenyl)-5-ethyl-4-methyl-1,3-oxazole 3-oxide | HCID 58284303 | — |
反応手順
1.00 g (8.69 mmol) of 2,3-pentanedione 2-oxime and 1.34 g (9.55 mmol) of 4-chlorobenzaldehyde are initially charged in 2 ml (34.94 mmol) of glacial acetic acid. With ice-cooling, hydrogen chloride gas is then introduced into the reaction mixture for 30 min. 10 ml of diethyl ether are then added to the reaction mixture. A precipitate is formed, which is filtered off with suction and washed twice with in each case 2 ml of diethyl ether. The precipitate is suspended in about 5 ml of water, and the suspension is made basic using aqueous ammonia. The suspension is then extracted four times with in each case 10 ml of dichloromethane. The combined organic phases are dried over magnesium sulphate, and the solvent is removed on a rotary evaporator. Without further purification, the product obtained in this manner is used for the subsequent step.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08653109B2 |
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| 出典データセット | uspto-grants-2014_02 |
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| ORD ID | ord-f7253a0df7cf486fa66a370b18d77029 |
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| 出典メモ | uspto-grants-2014_02 |
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