HuagongsheHuagongshe Chemistry Print Report · For research reference only
2,4-Difluoronitrobenzene → HCID 58707296, compound
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2,4-Difluoronitrobenzene | HCID 67967 | — |
| Reactant | Diisopropylethylamine | HCID 81531 | — |
| Reactant | Benzenemethanamine, 3,5-dichloro- | HCID 457602 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | HCID 58707296 | HCID 58707296 | 46% |
Reaction Steps
A mixture of 2,4-difluoronitrobenzene (5.0 mmol), 3,5-dichlorobenzylamine (5.0 mmol), N,N-diisopropylethylamine (10.0 mmol) and acetonitrile (25 mL) was heated at reflux for 18 h, cooled and concentrated in vacuo. The residue was dissolved in ethyl acetate; this solution was washed with water, dried over Na2SO4 and concentrated in vacuo. The residue was purified by flash column chromatography on silica gel using 5% ethyl acetate in hexanes as eluent to yield the title compound as a yellowish solid (46%). 1H NMR (400 MHz, CDCl3): δ 9.28 (br s, 1 H), 7.88 (m, 1 H), 7.34 (s, 1 H), 7.22 (s, 2 H), 6.44 (m, 1 H), 6.30 (dd, 1 H), 4.43 (d, 2 H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08604021B2 |
| Source dataset | uspto-grants-2013_12 |
| ORD ID | ord-9c11ed670cb64cbe9319d30759713ad4 |
| Source note | uspto-grants-2013_12 |