HuagongsheHuagongshe Chemistry Print Report · For research reference only
N-bromobutanimide → 3-Bromo-2,6-difluorobenzonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | N-bromobutanimide | HCID 67184 | — |
| Reactant | 2,6-Difluorobenzonitrile | HCID 74695 | — |
| Solvent | Sulfuric Acid | HCID 1118 | — |
| Product | 3-Bromo-2,6-difluorobenzonitrile | HCID 56604707 | — |
Reaction Steps
A solution of compound 2,6-difluorobenzonitrile (5 g, 36 mmol) in concentrated sulfuric acid (25 mL) was added with NBS (7 g, 39.6 mmol) at 0° C. and stirred at ambient temperature for 2 days. Ice was added to the reaction solution. The mixture was extracted with EtOAc. The organic layer was washed with water, saturated NaHCO3 solution, brine, dried over anhydrous sodium sulfate and concentrated. The residue was purified with fast column chromatograph to give compound 3-bromo-2,6-difluorobenzonitrile. 1H-NMR (400 MHz, CDCl3) δ ppm 7.78˜7.83 (m, 1H), 6.98˜7.03 (m, 1H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09056859B2 |
| Source dataset | uspto-grants-2015_06 |
| ORD ID | ord-c365ae0707414b11a737e0feea7c5b38 |
| Source note | uspto-grants-2015_06 |