HuagongsheHuagongshe Chemistry Print Report · For research reference only
Hydrochloric Acid → HCID 23139028, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Sodium Bicarbonate | HCID 516892 | — |
| Reactant | HCID 23139092 | HCID 23139092 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | HCID 23139028 | HCID 23139028 | — |
Reaction Steps
To a solution of (E)-4-(acetylsulfanyl)-1-[2-cyclopropyl-1-(2-fluorophenyl)-2-oxoethyl]-3-({2-[3-(ethoxycarbonyl)propyl]-2H-1,2,3-triazol-4-yl}methylidene)piperidine (570 mg) in ethanol (50 ml) was introduced HCl gas at 0° C. for 30 minutes. The mixture was stirred under tightly sealed condition for 2 hours, and the solvent and excess hydrogen chloride were removed in vacuo. The residue was purified by preparative HPLC (YMC-Pack ODS-A; YMC, eluent: acetonitrile/0.024 N HCl, 35/65, v/v) to afford a fraction containing the product. This fraction was treated with a saturated aqueous sodium hydrogen carbonate solution, and the liberated base was extracted with ethyl acetate to afford the free base of the title compound.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07829580B2 |
| Source dataset | uspto-grants-2010_11 |
| ORD ID | ord-ed04da0d3db94f238e910e0f7569d787 |
| Source note | uspto-grants-2010_11 |