反应详情

A 250 mL 2-neck flask fitted with a rubber septum, temperature probe, and addition funnel was charged with 2,4,5-trichloro-6-(5-chloro-2-methoxy-phenyl)-pyrimidine (5.97 g, 18.54 mmol) and CH2Cl2 (90 mL) and kept under a N2 atmosphere. BBr3 (1 M in CH2Cl2; 37.1 mL, 37.1 mmol, 2 equiv.) was added slowly via addition funnel so that the temperature never exceeded 25° C. After 1 h, water (90 mL) was added and the mixture was stirred for approximately 30 min. The organic layer was washed with satd. aq. NaHCO3, dried, and concentrated to give a yellow powder (5.6 g, 98%). MS (ESI+): mass calcd. for C10H5Cl4N2O, 308.9; m/z found, 308.9 [M+H]+. 1H NMR (CDCl3): 9.76 (s, 1H), 8.00 (d, J=2.6 Hz, 1H), 7.39 (dd, J=8.9, 2.6 Hz, 1H), 7.03 (d, J=8.9 Hz, 1H).

1. customA 250 mL 2-neck flask fitted with a rubber septum, temperature probe, and addition funnel
2. washThe organic layer was washed with satd
3. dry with materialaq. NaHCO3, dried
4. concentrationconcentrated