Participants
| Role | Name | HCID | Charge |
|---|
| Reactant | Hydrochloric Acid | HCID 313 | — |
| Reactant | Ethanol | HCID 702 | — |
| Reactant | HCID 86609425 | HCID 86609425 | — |
| Product | HCID 23138514 | HCID 23138514 | 68% |
Reaction Steps
Hydrogen chloride was passed through a solution of (E)-4-(acetylsulfanyl)-1-[2-cyclopropyl-1-(2-fluorophenyl)-2-oxoethyl]-3-({1-[2-(methoxycarbonyl)ethyl]-1H-1,2,3-triazol-5-yl}methylidene)piperidine hydrochloride (2.0 g) in ethanol (5.0 ml) with stirring at 0° C. for one hour, and the resulting mixture was stirred at room temperature under tightly sealed condition for 4 hours. After the reaction mixture was concentrated under reduced pressure, the residue was purified using preparative HPLC [YMC-Pack ODS-A; YMC, eluent: acetonitrile/0.024 N aqueous hydrochloric acid solution (33:67, v/v)]. The eluate was treated with hydrogen chloride (4 N dioxane solution, 2 ml). The solvent and excess hydrogen chloride were removed under reduced pressure to afford the title compound (1.29 g, yield: 68%) as a colourless amorphous solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|
| Patent number | US07829580B2 |
|---|
| Source dataset | uspto-grants-2010_11 |
|---|
| ORD ID | ord-b4dcd14bd8e84541a94ebecffe9ff6dc |
|---|
| Source note | uspto-grants-2010_11 |
|---|