참여 물질
| 역할 | 이름 | HCID | 투입량 |
|---|
| 반응물 | Water | HCID 962 | — |
| 반응물 | Dimethylformamide | HCID 6228 | — |
| 반응물 | Lithium iodide | HCID 66321 | — |
| 반응물 | Ethyl 2-acetylamino-2-(3-cyanobenzyl)malonate | HCID 22747914 | — |
| 용매 | Cyclohexane ethylacetate | HCID 21867204 | — |
| 생성물 | ethyl (2RS)-2-acetylamino-3-(3-cyanophenyl)propanoate | HCID 85797672 | — |
반응 단계
The process is performed as in Example 5, starting with 14.9 g of ethyl 2-acetylamino-2-(3-cyanobenzyl)malonate, 30 g of anhydrous lithium iodide and 150 cm3 of dry dimethylformamide. After stirring for 5 hours at a temperature in the region of 150° C., the reaction mass is cooled to room temperature. 1500 cm3 of water are added and the mixture is extracted with 3 times 300 cm of ethyl acetate. The extracts are combined, dried over magnesium sulfate, filtered and concentrated under reduced pressure (5 kPa) at a temperature in the region of 45° C. After drying in an oven at a temperature in the region of 40° C. under reduced pressure (10 Pa), 11.39 g of ethyl (2RS)-2-acetylamino-3-(3-cyanophenyl)propanoate are obtained in the form of a beige-colored paste. (Rf=0.51 in a 90/10 by volume mixture of ethyl acetate/cyclohexane, on a Merck 60F254R silica plate).
출처 및 근거
| DOI | 10.6084/m9.figshare.5104873.v1 |
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| 특허 번호 | US06699895B2 |
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| 출처 데이터셋 | uspto-grants-2004_03 |
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| ORD ID | ord-d79adc6f76f347a3a7b2f752585c18da |
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| 출처 메모 | uspto-grants-2004_03 |
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