HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 22253674, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethyl chloroformate | HCID 10928 | — |
| Reactant | HCID 22253670 | HCID 22253670 | — |
| Solvent | Acetone | HCID 180 | — |
| Product | HCID 22253674 | HCID 22253674 | 75.2% |
Reaction Steps
To a stirring mixture of 2-(2-bromo-propionylamino)-2-methyl-propionic acid (50.0 g; 0.21 mol), triethylamine (23.37 g; 0.23 mol) and 150 mL acetone, cooled with an ice bath, was added a solution of ethyl chloroformate (25.07 g; 0.23 mol) in 40 mL acetone 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 solid was washed with 150 mL ether. The combined filtrate was concentrated under vacuum. Ether (100 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 (63-64° C.; 1 mmHg) to give 34.73 g (75%) of a colorless oil.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06753391B1 |
| Source dataset | uspto-grants-2004_06 |
| ORD ID | ord-28ef0a4faf8c426b9f68996cb26bc645 |
| Source note | uspto-grants-2004_06 |