Triethylamine → HCID 22149514, compound

To a stirring mixture of 2-(2-chloro-acetylamino)-2-methyl propionic acid (18.0 g; 0.10 mol), triethylamine (11.1 g; 0.11 mol) and 100 mL acetone, cooled with an ice bath, was added ethyl chloroformate (10.5 mL; 0.11 mol) over a period of 10 minutes. The reaction mixture was then allowed to warm to room temperature and was stirred for 2 hours. The mixture was then filtered, and the filtrate was concentrated under vacuum. Hexane (200 mL) was added to the residue, and the mixture was filtered. After removal of the solvent under vacuum, the filtrate residue was distilled under reduced pressure (59-60° C.; 7 mmHg) to give 13.2 g (82%) of a colorless oil.

1. temperaturecooled with an ice bath
2. filtrationThe mixture was then filtered
3. concentrationthe filtrate was concentrated under vacuum
4. additionHexane (200 mL) was added to the residue
5. filtrationthe mixture was filtered
6. customAfter removal of the solvent under vacuum
7. distillationthe filtrate residue was distilled under reduced pressure (59-60° C.; 7 mmHg)

ORD record

ord-3039634c057f473e84414be7c9c5e09a

Source dataset

uspto-grants-2004_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06753391B1