Ethyl chloroformate → HCID 22149514, compound

To a stirring mixture of 2-(2-chloro-acetylamino)-2-methyl propionic acid (18.0 g; 0.100 mol), trichylamine (11.1 g; 0.110 mol) and 100 ml of acetone in a round bottom flask, cooled with an ice bath, was added ethyl chloroformate (10.5 ml; 0.110 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°; 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°; 7 mmHg)

ORD record

ord-49ce616fb97040e5adb83919385fc555

Source dataset

uspto-grants-2004_06

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US06747104B1