HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → HCID 86711945, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Ethoxalyl chloride | HCID 20884 | — |
| Reactant | HCID 66754828 | HCID 66754828 | — |
| Solvent | Water | HCID 962 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | HCID 86711945 | HCID 86711945 | 66% |
Reaction Steps
To a solution of 2-amino-1-(4-(trifluoromethoxy)phenyl)ethanone hydrochloride (9.5 g, 37 mmol) in DCM (150 mL) at 0° C. was added dropwise ethyl 2-chloro-2-oxoacetate (5.6 g, 41 mmol), followed by Et3N (16 mL, 111 mmol). The mixture was stirred at RT for 16 h and then diluted with H2O (200 mL) and extracted with EtOAc (4×80 mL). The combined organic layers were washed with brine (50 mL), dried over Na2SO4, filtered and concentrated under reduced pressure, and the residue was purified by silica gel column chromatography (Petroleum ether:EtOAc=5:1 to 1:1) to give the title compound as a yellow solid (7.8 g, 66%). MS (ES+) C13H12F3NO5 requires: 319. found: 320 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09018380B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-a8b3fb5619e842848e528325d35626d2 |
| Source note | uspto-grants-2015_04 |