反应详情

A mixture of 15.7 g (50 mmoles) of 1,3,5-tribromobenzene and 1.344 g (56 mmoles) of magnesium in 200 mL of THF was stirred 5 hrs. At room temperature 7.5 mL (100 mmoles) of DMF was then added at 0° and the reaction mixture was stirred overnight. Solvent was removed in vacuo at room temperature the residue was taken up in 200 mL of ethyl acetate and washed with 6×50 mL of satd. sodium chloride soln. The organic phase was dried over anhyd. MgSO4. Solvent was removed to give a crude solid, which was dissolved in minimum amount of methylene chloride, and applied on silica gel. Elution with 1:9 mixture of ether:hexane mixture containing 3% methylene chloride gave the desired 3,5-dibromobenzaldehyde as white solid.

1. stirringthe reaction mixture was stirred overnight
2. customSolvent was removed in vacuo at room temperature the residue
3. washwashed with 6×50 mL of satd
4. customThe organic phase was dried over anhyd
5. customSolvent was removed
6. customto give a crude solid, which
7. washElution
8. additionwith 1:9 mixture of ether
9. additionhexane mixture containing 3% methylene chloride