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-fb20914711cf4920a63f4f1857cd2c6c

Source dataset

uspto-grants-2005_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06911510B2