Ethanol → Ethyl 2-amino-2-methylpropanoate hydrochloride

Participants

Reaction Conditions

Reaction Steps

Ethanol (395 L) was added to 2-aminoisobutyric acid (79 Kg) and the mixture stirred at 20° C. Thionyl chloride (91.2 Kg) was added, maintaining the temperature at 540° C. The mixture was heated to reflux and stirred for 6 hours. The contents were distilled under atmospheric pressure to a residual volume of approximately 200 L over a period of 14 hours. The mixture was cooled to 45-50° C. and methyl tert-butyl ether (395 L) was added. The mixture was cooled to 0-5° C. and stirred for 1 hour. Material was isolated by filtration and washed with methyl tert-butyl ether (160 L) pre-cooled to 0-5° C., then dried in vacuo at 30-40° C. to give ethyl-2-aminoisobutyrate hydrochloride (105.5 Kg) with 86.2% purity in 71% yield (based on active).

Provenance & Evidence