HuagongsheHuagongshe Chemistry Print Report · For research reference only
Potassium Carbonate → 1-(3-Methoxy-4-nitrophenyl)-3,3-dimethylpiperidin-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Potassium Carbonate | HCID 11430 | — |
| Reactant | 5-Fluoro-2-nitroanisole | HCID 2779250 | — |
| Reactant | 3,3-Dimethylpiperidin-4-one | HCID 22278837 | — |
| Solvent | Dimethylformamide | HCID 6228 | — |
| Product | 1-(3-Methoxy-4-nitrophenyl)-3,3-dimethylpiperidin-4-one | HCID 58071496 | 43.6% |
Reaction Steps
4-Fluoro-2-methoxy-1-nitrobenzene (1.550 g, 9.06 mmol), 3,3-dimethylpiperidin-4-one (INTERMEDIATE 38) (2.17 g, 9.06 mmol, TFA salt), and potassium carbonate (2.504 g, 18.12 mmol) in DMF (20 ml) were heated at 70° C. overnight. The reaction mixture was concentrated in vacuo to remove the solvent. The residue was partitioned between CH2Cl2 (100 mL) and water (30 mL). The organic phase was dried over MgSO4 and concentrated in vacuo. The residue was purified using silica gel column (50%-100% CH2Cl2/Hexane) to obtain the title product (1.100 g, 43.6%).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08461170B2 |
| Source dataset | uspto-grants-2013_06 |
| ORD ID | ord-6b7d0eb2ec8a4d82947cc074fdd0a039 |
| Source note | uspto-grants-2013_06 |