반응 #76006
ord-d79adc6f76f347a3a7b2f752585c18da
반응 방정식
반응 조건
후처리
- 1온도the reaction mass is cooled to room temperature
- 2추출the mixture is extracted with 3 times 300 cm of ethyl acetate
- 3건조dried over magnesium sulfate
- 4여과filtered
- 5농축concentrated under reduced pressure (5 kPa) at a temperature in the region of 45° C
- 6건조After 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
- 7기타are obtained in the form of a beige-colored paste
실험 절차
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).