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HRID 47728作成日:2026年10月24日

Water → ethyl (2RS)-2-acetylamino-3-(3-cyanophenyl)propanoate

https://huagongshe.com/ja/reaction/47728

反応式

関与物質

役割名称HCID仕込み量
反応物WaterHCID 962—
反応物DimethylformamideHCID 6228—
反応物Lithium iodideHCID 66321—
反応物Ethyl 2-acetylamino-2-(3-cyanobenzyl)malonateHCID 22747914—
溶媒Cyclohexane ethylacetateHCID 21867204—
生成物ethyl (2RS)-2-acetylamino-3-(3-cyanophenyl)propanoateHCID 85797672—

反応条件

温度150 °C

反応手順

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).

情報源と証拠

DOI10.6084/m9.figshare.5104873.v1
特許番号US06699895B2
出典データセットuspto-grants-2004_03
ORD IDord-d79adc6f76f347a3a7b2f752585c18da
出典メモuspto-grants-2004_03