HuagongsheHuagongshe Chemistry Print Report · For research reference only
2-Bromo-3-nitro-5-(trifluoromethyl)pyridine → 3-Nitro-5-(trifluoromethyl)picolinonitrile
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 2-Bromo-3-nitro-5-(trifluoromethyl)pyridine | HCID 46315200 | — |
| Reactant | HCID 178418546 | HCID 178418546 | — |
| Catalyst | Tetrabutylammonium Bromide | HCID 74236 | — |
| Solvent | Toluene | HCID 1140 | — |
| Product | 3-Nitro-5-(trifluoromethyl)picolinonitrile | HCID 45382147 | — |
Reaction Steps
2-Bromo-3-nitro-5-trifluoromethyl-pyridine (10.00 g, 36.87 mmol) was dissolved in toluene (250 ml) with stirring to give a pale yellow solution. Tetrabutylammonium bromide (11.90 g, 36.9 mmol) was added followed by copper(I) cyanide (9.92 g, 111 mmol) and the mixture was heated at reflux for 10 h. After cooling to RT, the reaction mixture was partitioned between water (750 ml) and EtOAc (750 ml). The organic fractions were combined, washed with water (2×250 ml) and brine (100 ml), dried (MgSO4) and concentrated in vacuo to afford the title product. 1H-NMR: [400 MHz, DMSO-d6 δH 9.55 (1H, m, ArH), 9.24 (1H, m, ArH)
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US08476269B2 |
| Source dataset | uspto-grants-2013_07 |
| ORD ID | ord-1432742050b14b79a454a3a11fc3e088 |
| Source note | uspto-grants-2013_07 |