HuagongsheHuagongshe Chemistry Print Report · For research reference only
Sodium Hydroxide → 351407-14-2
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Sodium Hydroxide | HCID 14798 | — |
| Reactant | Thionyl Chloride | HCID 24386 | — |
| Reactant | HCID 22678292 | HCID 22678292 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 351407-14-2 | HCID 22678296 | 83.3% |
Reaction Steps
6.09 g of 1-[(2-methoxy-3-pyridyl)methyl]-4-[2-(3-methylsulfonyl-2-thienyl)ethyl]piperidine obtained in Example 43 and 2 ml of thionyl chloride were dissolved in 50 ml of ethanol, and the mixture was heated under reflux for 2 hours. The reaction mixture was basified by adding a 1N aqueous sodium hydroxide thereto, and then extracted with dichloromethane. The organic layer was washed with brine, and then dried over anhydrous magnesium sulfate. The solvent was evaporated, and the resulting crude product was purified by NH form silica gel column chromatography (ethyl acetate), to give 4.89 g of the title compound as colorless crystals.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US06784192B2 |
| Source dataset | uspto-grants-2004_08 |
| ORD ID | ord-00ca5ea8d27945e7b67f204378a39566 |
| Source note | uspto-grants-2004_08 |