HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ammonium Chloride → HCID 68551762, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ammonium Chloride | HCID 25517 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-Chloro-3-(trifluoromethyl)pyridine | HCID 589833 | — |
| Reactant | HCID 5190868 | HCID 5190868 | — |
| Solvent | 1,4-Dioxane | HCID 31275 | — |
| Product | HCID 68551762 | HCID 68551762 | 55% |
Reaction Steps
To a microwave vial were charged 4-(phenylsulfonyl)piperidine (300 mg, 1.33 mmol), 2-chloro-3-(trifluoromethyl)pyridine, (484 mg, 2.66 mmol), diisopropylethylamine (0.695 mL, 3.99 mmol) and 1,4-Dioxane (0.2 mL). The reaction mixture thus prepared was irradiated at 200° C. for 1 hour. The reaction was complete as determined by TLC. The residue was added with saturated NH4Cl (aq.) and extracted with ethylacetate, washed with 10% HCl (aq.), water then brine. Organic layer was dried over MgSO4. Solvent evaporation afforded 2-[4-(phenylsulfonyl)piperidin-1-yl]-3-(trifluoromethyl)pyridine in 55% yield (270 mg) as white solid.
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07632838B2 |
| Source dataset | uspto-grants-2009_12 |
| ORD ID | ord-570587f1a97d462da435cce6022d79cd |
| Source note | uspto-grants-2009_12 |