HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 69080162, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Dichloromethane | HCID 6344 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 69081459 | HCID 69081459 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 69080162 | HCID 69080162 | — |
Reaction Steps
A solution of ethyl 2-(2-fluoro-6-methoxyphenyl)-4,5-dioxo-1-(4-(trifluoromethoxy)benzyl)pyrrolidine-3-carboxylate (2.937 g; 6.26 mmol) in dioxane (13 ml) was treated with 25% hydrochloric acid (13 ml). The resulting mixture was then refluxed, under nitrogen, for 11 h. After cooling to rt, DCM and aq. sat. NaHCO3 were added. The separated aqueous layer was further extracted with DCM. The mixed organic layers were washed with brine, dried over anh. MgSO4, filtered, and concentrated to dryness under reduced pressure affording 5-(2-fluoro-6-methoxyphenyl)-1-(4-(trifluoromethoxy)benzyl)pyrrolidine-2,3-dione which was used for the next step without additional purification. LC-MS (conditions A): tR=0.85 min.; [M+H]+: 397.99 g/mol.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09242970B2 |
| Source dataset | uspto-grants-2016_01 |
| ORD ID | ord-cc5cdbf36fad44c0b9b00777c6f762ad |
| Source note | uspto-grants-2016_01 |