反应 #2971024
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openreactiondata ↗doi:10.6084/m9.figshare.5104873.v1; patent:US08871304B2
反应条件: temp:0.00; pressure:0.00; stir:; See reaction.notes.procedure_details.
实验步骤: Into a 50 mL-volume flask equipped with a stirrer, a thermometer and a dropping funnel were placed 6.0 g (0.10 mol) of isopropylamine and 5 ml of water. And then, while maintaining the solution temperature within a range of from 30° C. to 50° C., 10 ml of aqueous solution of 5.0 g (35 mmol) of 2-(dimethylamino)ethyl chloride hydrochloride was slowly dropped into the flask, and the mixture was stirred for 2 hours. Subsequently, 10 ml of aqueous solution of 2.8 g (70 mmol) of sodium hydroxide was slowly dropped into the flask in an ice bath, and the mixture was reacted for 10 minutes. After the completion of the reaction, the reaction solution was subjected to extraction with 25 ml of hexane twice, and the hexane layer was concentrated under reduced pressure. The resultant concentrate was distilled under reduced pressure (65° C., 4.0 kPa), to provide 1.4 g of 1-isopropylamino-2-dimethylaminoethane. (Isolation yield: 31%) Into a 50 mL-volume flask equipped with a stirrer was slowly dropped into the flask the mixture was reacted for 10 minutes After the completion of the reaction the reaction solution was subjected to extraction with 25 ml of hexane twice the hexane layer was concentrated under reduced pressure The resultant concentrate was distilled under reduced pressure (65° C., 4.0 kPa)
来源 ID: ord-0bdd27d8e9754321b22be4bcd5ef600e