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-Butanedione monoxime | HCID 6409633 | — |
| 溶媒 | Diethyl Ether | HCID 3283 | — |
| 生成物 | 2-(4-Chlorophenyl)-4,5-dimethyl-1,3-oxazol 3-oxide | HCID 3243952 | — |
反応手順
1.00 g (9.89 mmol) of diacetylmonoxime and 1.53 g (10.88 mmol) of 4-chlorobenzaldehyde are initially charged in 2 ml (34.94 mmol) of glacial acetic acid. With ice-cooling of the reaction mixture, hydrogen chloride gas is then introduced 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 resuspended in about 5 ml of water and the suspension is made basic using ammonia. The mixture is then extracted four times with in each case 10 ml of dichloromethane. The combined organic phases are dried over magnesium sulfate and the solvent is removed on a rotary evaporator. The residue is used in the next reaction without further purification.
情報源と証拠
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 特許番号 | US08304412B2 |
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| 出典データセット | uspto-grants-2012_11 |
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| ORD ID | ord-0efbddccaff645478b0fec6f552c813a |
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| 出典メモ | uspto-grants-2012_11 |
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