HuagongsheHuagongshe Chemistry Print Report · For research reference only
Diisopropylethylamine → N-(6-Methoxypyridin-3-yl)-4-(2-methylphenoxy)piperidine-1-carbothioamide
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 5-Isothiocyanato-2-methoxypyridine | HCID 12666025 | — |
| Reactant | 4-(2-Methylphenoxy)piperidine hydrochloride | HCID 17178056 | — |
| Solvent | Dichloromethane | HCID 6344 | — |
| Product | N-(6-Methoxypyridin-3-yl)-4-(2-methylphenoxy)piperidine-1-carbothioamide | HCID 57753857 | 85% |
Reaction Steps
5-Isothiocyanato-2-methoxypyridine [(829 mg, 4.99 mmol), J. Org. Chem. (1980), 45, 4219] was added to a solution of 4-(2-methylphenoxy)-piperidine hydrochloride [(990 mg, 4.3 mmol), J. Med. Chem. (1978), 21, 309] and N,N-diisopropylethylamine (0.79 mL, 4.7 mmol) in dichloromethane (10 mL) and the mixture was stirred for 3 hours at room temperature. The organic solution was then diluted with dichloromethane and washed with sodium hydrogen carbonate solution and brine. The organic solution was dried over magnesium sulfate and concentrated in vacuo. Trituration of the residue with diethyl ether afforded the title compound as a solid in 85% yield, 1.3 g. LRMS APCI m/z 358 [M+H]+
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08207198B2 |
| Source dataset | uspto-grants-2012_06 |
| ORD ID | ord-46b40954c91f42c698693e3b1acca279 |
| Source note | uspto-grants-2012_06 |