反应详情

温度

0 °C

To a suspension of lead thiocyanate (6.49 g, 20.05 mmol) in CH2Cl2 (125 mL) under nitrogen at 0° C. PhICl2 (4.41 g, 16.05 mmol) was added in one portion. After 20 min at 0° C. a solution of 2-bromophenol (2.31 g, 1.55 mL, 13.37 mmol) in CH2Cl2 (10 mL) was added. After stirring the mixture for 45 min at 0° C. the salts were filtered and the solvent evaporated. The crude mixture was purified by silica gel flash chromatography (hexane-EtOAc 5:1→2:1) to yield 1 (2-bromo4-thiocyanatophenol) (1031 mg, 33%) as a pale yellow oil.

1. additionPhICl2 (4.41 g, 16.05 mmol) was added in one portion
2. filtrationwere filtered
3. customthe solvent evaporated
4. customThe crude mixture was purified by silica gel flash chromatography (hexane-EtOAc 5:1→2:1)