Diethylamine → HCID 18435495, compound

Temperature

0 °C

N-(t-Butyloxycarbonyl)-β-alanine, 3.8 g (20 mmol) was dissolved in 50 ml of tetrahydrofuran, and the solution was cooled to 0° C. and stirred. To this mixture, 2.4 g (24 mmol) of triethylamine was added and 2.16 g (20 mmol) of ethyl chloroformate was slowly added. After stirring the reaction mixture for an hour at 0° C., 4 ml of 40% diethylamine aqueous solution was slowly added and stirred vigorously for an hour. The mixture was extracted by adding 100 ml of dichloromethane and 50 ml of water. The organic layer was washed with 1 N HCl aqueous solution and subsequently with saturated sodium bicarbonate aqueous solution. The washed mixture was dried to obtain 3.9 g (90%) of N-(t-butyloxy-carbonyl)-β-alanine dimethylamide.

1. stirringAfter stirring the reaction mixture for an hour at 0° C.
2. stirringstirred vigorously for an hour
3. extractionThe mixture was extracted
4. additionby adding 100 ml of dichloromethane and 50 ml of water
5. washThe organic layer was washed with 1 N HCl aqueous solution and subsequently with saturated sodium bicarbonate aqueous solution
6. customThe washed mixture was dried

ORD record

ord-8efd0da1fb434eb3a94a4ea6d2cbd383

Source dataset

uspto-grants-2002_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06436921B1