참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Acetic Acid | HCID 176 | — |
| 반응물 | Hydrochloric Acid | HCID 313 | — |
| 반응물 | 4-Chlorobenzaldehyde | HCID 7726 | — |
| 반응물 | 2,3-Pentanedione, 2-oxime | HCID 6797453 | — |
| 용매 | Diethyl Ether | HCID 3283 | — |
| 생성물 | 2-(4-Chlorophenyl)-5-ethyl-4-methyl-1,3-oxazole 3-oxide | HCID 58284303 | — |
반응 단계
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.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US08653109B2 |
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| 출처 데이터셋 | uspto-grants-2014_02 |
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| ORD ID | ord-f7253a0df7cf486fa66a370b18d77029 |
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| 출처 메모 | uspto-grants-2014_02 |
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