HuagongsheHuagongshe Chemistry Print Report · For research reference only
Triethylamine → 1-(2,6-Difluoro-4-nitrophenyl)piperidin-4-one
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Triethylamine | HCID 8471 | — |
| Reactant | Piperonylamine | HCID 2723901 | — |
| Reactant | 1,2,3-Trifluoro-5-nitrobenzene | HCID 2782793 | — |
| Solvent | Chloroform | HCID 6212 | — |
| Product | 1-(2,6-Difluoro-4-nitrophenyl)piperidin-4-one | HCID 21878183 | 94% |
Reaction Steps
To a mixture of 3,4,5-trifluoronitrobenzene (3.894 g, 0.022 mol) and 4-piperidone hydrochloride monohydrate (3.072 g, 0.020 mol) in chloroform (24 ml), was added triethylamine (8.3 ml, 0.06 mol) under stirring. The resulting mixture was heated and stirred at 70° C. for 7 h. After completion of the reaction (TLC), the solvent was evaporated under reduced pressure and the residue diluted with water (10 ml). The separated solid was filtered, washed with water (8 ml) followed by hexane (5 ml) to obtain yellow crystalline solid as a product, 4.8 g, 94% yield M.P.: 130-132° C.; MS: M+1=257 (MH+ 100%) for M.F.: C11H10F2N2O3
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08217058B2 |
| Source dataset | uspto-grants-2012_07 |
| ORD ID | ord-fa38bc2ed7aa4e96a0d24a7e09bb80a9 |
| Source note | uspto-grants-2012_07 |