HuagongsheHuagongshe Chemistry Print Report · For research reference only
HCID 86711945, compound → HCID 86711946, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | HCID 86711945 | HCID 86711945 | — |
| Solvent | Phosphorus oxychloride | HCID 24813 | — |
| Product | HCID 86711946 | HCID 86711946 | 87.1% |
Reaction Steps
A solution of ethyl 2-oxo-2-(2-oxo-2-(4-(trifluoromethoxy)phenyl)ethylamino)acetate (7.8 g, 24.4 mmol) in POCl3 (50 mL) was heated at 110° C. for 3 h, and then cooled to RT. The mixture was concentrated under reduced pressure, diluted with ice—H2O (100 mL) and extracted with EtOAc (3×50 mL). The combined organic layers were washed with H2O (2×50 mL), brine (30 mL), dried over Na2SO4, filtered and concentrated under reduced pressure. The residue was purified by silica gel column chromatography (Petroleum ether:EtOAc=5:1 to 2:1) to give the title compound as a light yellow solid (6.4 g, 87%). MS (ES+) C13H10F3NO4 requires: 301. found: 302 [M+H]+.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09018380B2 |
| Source dataset | uspto-grants-2015_04 |
| ORD ID | ord-827647147d19496faf0ddfa10448c8f7 |
| Source note | uspto-grants-2015_04 |