HuagongsheHuagongshe Chemistry Print Report · For research reference only
Nitrogen → (4-Bromo-2-chlorophenyl)acetonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Nitrogen | HCID 947 | — |
| Reactant | Trimethylsilyl cyanide | HCID 82115 | — |
| Reactant | Tetrabutylammonium Fluoride | HCID 2724141 | — |
| Reactant | 4-Bromo-1-(bromomethyl)-2-chlorobenzene | HCID 21914486 | — |
| Solvent | Acetonitrile | HCID 6342 | — |
| Product | (4-Bromo-2-chlorophenyl)acetonitrile | HCID 58762522 | 80.3% |
Reaction Steps
4-Bromo-1-bromomethyl-2-chloro-benzene (3.04 g, 10.7 mmoles) was dissolved into anhydrous CH3CN. To this mixture (under N2 at ambient temp) was added TMSCN (2.1 mL, 15.7 mmoles) followed by 1.0M TBAF (15.7 mL, 15.7 mmoles, soln in THF). The resulting mixture was stirred at ambient temperature for 15 min after which time it was evaporated in vacuo to yield crude residue. The crude residue was purified using flash silica chromatography (0-10% EtOAc/Hexane) to yield (4-bromo-2-chloro-phenyl)-acetonitrile (1.98 g, 80%) as an off-white solid. 1H-NMR (CDCl3): δ 7.60 (d, J=2.0 Hz, 1H), 7.47 (dd, J′=8.1 Hz, J″=1.8 Hz, 1H), 7.39 (d, J=8.1 Hz, 1H), 3.79 (s, 2H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08013001B2 |
| Source dataset | uspto-grants-2011_09 |
| ORD ID | ord-1852eac9037c42328e40a5dbf8f960e7 |
| Source note | uspto-grants-2011_09 |