HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1-(3-Methyl-1,2,4-thiadiazol-5-yl)piperidin-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | 4-Piperidone hydrochloride | HCID 3084851 | — |
| Reactant | 5-Chloro-3-methyl-1,2,4-thiadiazole | HCID 12919159 | — |
| Solvent | Ethanol | HCID 702 | — |
| Product | 1-(3-Methyl-1,2,4-thiadiazol-5-yl)piperidin-4-one | HCID 59258510 | 8.6% |
Reaction Steps
To a mixture of piperidin-4-one HCl salt (C3) (4.08 g, 30 mmol) and Et3N (20 mL, 78.6 mmol) in EtOH (50 mL) was added 5-chloro-3-methyl-1,2,4-thiadiazole (4.05 g, 30 mmol). The mixture was heated to reflux for 1.5 h and then concentrated to dryness. The residue was dissolved in EtOAc. The solution was washed with water (30 mL×3) and brine (30 mL), dried over Na2SO4, and concentrated to dryness. The residue was recrystallized from ether to give 1-(3-methyl-1,2,4-thiadiazol-5-yl)piperidin-4-one (D1) (510 mg). 1H-NMR (300 MHz, CDCl3) δ 3.86 (t, J=6.3 Hz, 4H), 2.62 (t, J=6.3, Hz, 4H), 2.44 (s, 3H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US07696201B2 |
| Source dataset | uspto-grants-2010_04 |
| ORD ID | ord-793571c76f1e4385a26b64a8c6545c4a |
| Source note | uspto-grants-2010_04 |