反应详情

To a solution of 2-benzyloxy-4-chloro-3-nitro-pyridine (Wilde, et al. WO 99/01454, which is incorporated herein by reference) (6.59 g, 24.9 mmol) in DME/H2O, was added 2-chloro-4-difluoromethoxy-phenylboronic acid (Wilde, et al. WO 99/01454) (5.54 g, 24.9 mmol), Ba(OH)2 8H2O (7.86 g, 24.9 mmol), and Pd(PPh3)2Cl2 (1.01 g, 1.45 mmol) and the mixture was heated at reflux for 5 h. The reaction was cooled and poured into EtOAc and H2O (500 mL). The EtOAc layer was washed with H2O, brine, dried Na2SO4, filtered and concentrated in vacuo to give 6.9 g (68%) of 2-benzyloxy-4-(2-chloro-4-difluoromethoxy-phenyl)-3-nitro-pyridine as a viscous oil; MS(AP) m/z 408.9 [(M+H)+, 100].

1. temperaturethe mixture was heated
2. temperatureat reflux for 5 h
3. temperatureThe reaction was cooled
4. washThe EtOAc layer was washed with H2O, brine, dried Na2SO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo