HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → 2-(4-Carboxymethylamino-3-fluorophenyl)-6,8-difluoro-5-hexylamino-4H-1-benzopyran-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Water | HCID 962 | — |
| Reactant | 2-[4-(N-acetyl-N-ethoxycarbonylmethylamino)-3-fluorophenyl]-6,8-difluoro-5-hexylamino-4H-1-benzopyran-4-one | HCID 19434976 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | 2-(4-Carboxymethylamino-3-fluorophenyl)-6,8-difluoro-5-hexylamino-4H-1-benzopyran-4-one | HCID 19434985 | 77% |
Reaction Steps
143 mg (0.276 mmol) of Compound 74 obtained in Example 74 was dissolved in 12 ml of dioxane, 8 ml of concentrated hydrochloric acid was added and the mixture was heated ar reflux for 10 minutes. The reaction solution was cooled on ice, water was added and the mixture was extracted with ethyl acetate. The organic layer was washed twice with water and once with an aqueous saturated solution of sodium chloride and dried over anhydrous sodium sulfate, and the solvent was distilled off under reduced pressure. The residue was recrystallized from ethyl acetate/n-hexane to give 95 mg (77%) of Compound 75.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05539112 |
| Source dataset | uspto-grants-1996_07 |
| ORD ID | ord-7012fb3a54b6483a9cdf13bbea0d21c5 |
| Source note | uspto-grants-1996_07 |