참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Toluene | HCID 1140 | — |
| 반응물 | Morpholine | HCID 8083 | — |
| 반응물 | 4-Ethylcyclohexanone | HCID 79506 | — |
| 반응물 | p-Toluenesulfonic acid monohydrate | HCID 521998 | — |
| 생성물 | (5-Ethyl-2-morpholin-4-yl-cyclohex-2-enylidene)-acetic acid ethyl ester | HCID 66883521 | — |
반응 단계
91.6 g of 4-Ethyl-cyclohexanone, 73.6 g of morpholine and 2 g of p-toluene-sulfonic acid monohydrate are dissolved in 400 ml of toluene. The mixture is heated to reflux and the water formed is removed by a water separator. After reacting for about 24 h, the reaction mixture is cooled to 100° C. and 2 g of p-toluene-sulfonic acid are added, followed by the addition of 157.22 g of glyoxylic acid ethyl ester during 30 minutes. The mixture is again heated to reflux for 5 hours and allowed to cool down to 22° C. The solvent is evaporated in vacuo and the crude product is distilled in vacuo at 140-150° C./9.5−2 mbar.
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US07906677B2 |
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| 출처 데이터셋 | uspto-grants-2011_03 |
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| ORD ID | ord-56376add803b45279b12c1ab4a728805 |
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| 출처 메모 | uspto-grants-2011_03 |
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