反应详情

温度

90 °C

To the solution of 3-bromo-5-ethoxy-4-hydroxybenzaldehyde (1.00 g, 4.08 mmol) in pyridine (10 mL) was added Cu powder (0.52 g, 8.1 mmol) and methyl disulfide (0.77 g, 8.2 mmol), the mixture was then heated at 90° C. overnight. The reaction mixture was filtered, and the solvent was removed under reduced pressure, the residue was poured into water, and 6 N HCl (5 mL) was added, then the mixture was extracted with DCM (50 mL×3), the combined organic layers were washed with brine, dried over Na2SO4 and concentrated. The residue was purified by silica gel column (PE:EA=5:1) to give Intermediate 50 (600 mg, yield 69%).

1. filtrationThe reaction mixture was filtered
2. customthe solvent was removed under reduced pressure
3. additionthe residue was poured into water, and 6 N HCl (5 mL)
4. additionwas added
5. extractionthe mixture was extracted with DCM (50 mL×3)
6. washthe combined organic layers were washed with brine
7. dry with materialdried over Na2SO4
8. concentrationconcentrated
9. customThe residue was purified by silica gel column (PE:EA=5:1)