Isopropylamine → N~1~,N~1~-Dimethyl-N~2~-(propan-2-yl)ethane-1,2-diamine

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%)

1. customInto a 50 mL-volume flask equipped with a stirrer
2. additionwas slowly dropped into the flask
3. customthe mixture was reacted for 10 minutes
4. customAfter the completion of the reaction
5. extractionthe reaction solution was subjected to extraction with 25 ml of hexane twice
6. concentrationthe hexane layer was concentrated under reduced pressure
7. concentrationThe resultant concentrate
8. distillationwas distilled under reduced pressure (65° C., 4.0 kPa)

ORD record

ord-0bdd27d8e9754321b22be4bcd5ef600e

Source dataset

uspto-grants-2014_10

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08871304B2