反应详情

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 9 hrs. 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] δ 9.55 (1H, m, ArH), 9.24 (1H, m, ArH)

1. customto give a pale yellow solution
2. temperaturethe mixture was heated
3. temperatureat reflux for 9 hrs
4. customthe reaction mixture was partitioned between water (750 ml) and EtOAc (750 ml)
5. washwashed with water (2×250 ml) and brine (100 ml)
6. dry with materialdried (MgSO4)
7. concentrationconcentrated in vacuo