HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23086711, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | HCID 23086679 | HCID 23086679 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 23086711 | HCID 23086711 | 5.4% |
Reaction Steps
Ethyl 5-hydroxy-3-(3-trifluoromethylphenyl)-5,6,7,8-tetrahydrocinnoline-7-carboxylate (60 mg, 0.164 mmol) obtained in Example 3 was dissolved in dioxane (1 mL), followed by adding 0.1 ml of a concentrated HCl solution and stirring over night. The reaction liquid was concentrated, followed by neutralization with an aqueous solution of sodium hydrogen carbonate, making weak acid using a 1N aqueous solution of sodium hydrogen sulfate, extraction with ethyl acetate, drying with sodium sulfate anhydride, filtration, concentration of thus obtained organic layer under reduced pressure and purification of residue using silica gel column chromatography (methylene chloride/methanol=10/1) to obtain an objective compound (3 mg, 5.4%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07563893B2 |
| Source dataset | uspto-grants-2009_07 |
| ORD ID | ord-5caf36383a174e629e572ba09ab5645c |
| Source note | uspto-grants-2009_07 |