反应详情

温度

-78 °C

To a stirred solution of 4-bromo-3-methylbenzonitrile (4.0 g, 20 mmol) in 100 mL of anhydrous THF was added BuLi (1.6 M, 12.8 mL) dropwise at −78° C. under nitrogen atmosphere. After the addition, the pale red solution was stirred for 5 min at −78° C. and dry DMF (2.2 mL) then added drop wise. After 20 min, the reaction mixture was poured onto a saturated solution of sodium chloride (100 mL). The organic phase was separated, extracted with diethyl ether (100 mL), dried over Na2SO4 and distilled off the solvent to afford 3.5 g of crude 4-formyl-3-methylbenzonitrile. MS m/z: 146 (M+1)+.

1. additionAfter the addition
2. waitAfter 20 min
3. customThe organic phase was separated
4. extractionextracted with diethyl ether (100 mL)
5. dry with materialdried over Na2SO4
6. distillationdistilled off the solvent