HuagongsheHuagongshe Chemistry Print Report · For research reference only
Acetic Acid Mixture with Hydrobromic Acid → HCID 86648761, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Acetic Acid Mixture with Hydrobromic Acid | HCID 21893785 | — |
| Reactant | HCID 86648760 | HCID 86648760 | — |
| Solvent | Acetic Acid | HCID 176 | — |
| Solvent | Ethyl Acetate | HCID 8857 | — |
| Product | HCID 86648761 | HCID 86648761 | 59% |
Reaction Steps
Methyl cis(±)-5-(4-{[(benzyloxy)carbonyl]amino}-3-methoxypiperidin-1-yl)-2-methylthiophene-3-carboxylate obtained in Example (188c) (50 mg) was dissolved in acetic acid (1 mL). A hydrobromic acid-acetic acid solution (1 ml) was added, and the mixture was stirred at room temperature for one hour. The reaction solution was diluted with ethyl acetate, washed with water and brine, and dried over anhydrous sodium sulfate. Following concentration under reduced pressure, the residue was purified by silica gel column chromatography (elution solvent: methanol/ethyl acetate=0, 10%) to obtain 20 mg of the title compound as a glassy solid (59%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08536197B2 |
| Source dataset | uspto-grants-2013_09 |
| ORD ID | ord-156ed93175834bcead88774dca9f4d4e |
| Source note | uspto-grants-2013_09 |