HuagongsheHuagongshe Chemistry Print Report · For research reference only
Ethylamine → HCID 68157886, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Ethylamine | HCID 6341 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | 2-(2,6-Difluoro-3-nitrophenyl)pyridine | HCID 14419433 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 68157886 | HCID 68157886 | 90% |
Reaction Steps
2-(2,6-Difluoro-3-nitrophenyl)pyridine (1.00 g, 4.29 mmol), ethylamine (2.24 mL, 4.29 mmol) and then DIPEA (0.75 mL, 4.29 mmol) were added to acetonitrile (10 mL) and the resultant mixture stirred at 20° C. for 40 hours under a nitrogen atmosphere. The mixture was concentrated in vacuo and the residue was purified by silica gel chromatography (Si—PPC, gradient 0-50% EtOAc/cyclohexane) to give the title compound as yellow oil (1.00 g, 90%). 1H NMR (CDCl3) δ: 8.73 (1H, ddd, J=6.6, 2.4, 1.3 Hz), 8.28 (1H, dd, J=12.6, 8.1 Hz), 7.80 (1H, td, J=10.3, 2.4 Hz), 7.45 (1H, dq, J=10.4, 1.6 Hz), 7.33 (1H, ddd, J=10.1, 6.5, 1.6 Hz), 6.51 (1H, dd, J=12.7, 10.9 Hz), 2.54-2.44 (2H, m), 1.03 (3H, t, J=9.6 Hz)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08653089B2 |
| Source dataset | uspto-grants-2014_02 |
| ORD ID | ord-05b44a658fd84270a50bad69166465a6 |
| Source note | uspto-grants-2014_02 |