反应详情

Dissolve (2,6-dichloro-4-methoxy-phenyl)-methanol (113 g, 545.76 mmol) in 1200 mL dry THF and cool to 0 deg under nitrogen. Add PBr3 (59.1 g, 218.3 mmol) under nitrogen and stir at 0° C. for 30 minutes. Pour into saturated aqueous NaHCO3 and extract with EtOAc. Dry and concentrate under vacuum to obtain 129.4 g product as an off-white solid. NMR (CDCl3) δ 6.88 (s, 2H), 4.73 (s, 2H), 3.79 (s, 3H).

1. temperaturecool to 0 deg under nitrogen
2. extractionextract with EtOAc
3. customDry
4. concentrationconcentrate under vacuum