反应详情

To ice cold conc. sulphuric acid (400 mL) was added fuming nitric acid (200 mL) dropwise followed by 3-bromobenzaldehyde (i) (100 g, 0.540 mol) dropwise over 15 min. The reaction mixture was stirred for 10 min and then poured carefully over ice-water. The resulting solids were filtered and then purified by flash column chromatography on silica gel, eluting with EtOAc:n-hexane (gradient elution from 1% to 20% v/v) to give (ii) (60 g, 48%).

1. filtrationThe resulting solids were filtered
2. custompurified by flash column chromatography on silica gel
3. washeluting with EtOAc
4. washn-hexane (gradient elution from 1% to 20% v/v)