참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Chlorobenzaldehyde | HCID 7726 | — |
| 반응물 | 2,3-Butanedione monoxime | HCID 6409633 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 2-(4-Chlorophenyl)-4,5-dimethyl-1,3-oxazol 3-oxide | HCID 3243952 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08304412B2 |
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| 출처 데이터셋 | uspto-grants-2012_11 |
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| ORD ID | ord-0efbddccaff645478b0fec6f552c813a |
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| 출처 메모 | uspto-grants-2012_11 |
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