反应详情

To POCl3 (7.5 ml, 80 mmol) was added in portions solid 6 (2.25 g, 10 mmol). The mixture was stirred at room temperature for 30 min and then 60° C. for 10 min. The mixture was then poured into cold 1M NaOH extracted with CH2C2. The combined extracts were dried (K2CO3) and concentrated to a residue which was purified by flash chromatography (EtOAc) to afford 3-Bromo-2-chloroquinoline 7 (1.95 g, 80%). 1H NMR d (ppm): 7.6 dd (CH atom), 7.7 m (2 CH atom), 8.0 d (CH atom), 8.5 s (CH arom)

1. wait60° C. for 10 min
2. extractionextracted with CH2C2
3. dry with materialThe combined extracts were dried (K2CO3)
4. concentrationconcentrated to a residue which
5. customwas purified by flash chromatography (EtOAc)