HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 10959481, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Potassium tert-butoxide | HCID 23665647 | — |
| Reactant | HCID 86756351 | HCID 86756351 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | HCID 10959481 | HCID 10959481 | 83% |
Reaction Steps
The crude 3-[[2-[(5-chloro-2-hydroxyphenyl)carbonyl]-4-(trifluoromethyl)phenyl]amino]-3-oxopropanoic acid, methyl ester prepared in Step B was dissolved in THF (15 mL) and potassium t-butoxide solution (1M in THF, 1.74 mmol, 1.74 mL) was added. The reaction mixture was heated under reflux for 15 minutes. It was then acidified with 1N HCl and the organic layer was separated. The organic layer was washed with water, brine and dried (MgSO4). Evaporation of the solvent gave a yellow solid which was triturated with ethyl acetate/hexanes to afford the title compound as a yellow solid (0.48 g, 83%): mp>250° C. MS m/e 366 (MH+).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06184231B2 |
| Source dataset | uspto-grants-2001_02 |
| ORD ID | ord-5d4e1cc32a0d473ebf27ff22843cf0c7 |
| Source note | uspto-grants-2001_02 |