反应详情

温度

0 °C

0.73 g of 4-(4-methyl-piperazin-1-yl-methyl)-benzonitrile (3.40 mmol) were dissolved in toluene (13 ml) and added to a solution of 3 M methyl magnesium bromide in diethyl ether (3.4 ml, 10.2 mmol) under nitrogen atmosphere. The resulting suspension was heated under reflux for 4 hours. The reaction was cooled down to 0° C., acidified with 10% HCl and then heated under reflux for 1 hour. The two phases were separated and the aqueous phase rinsed with AcOEt, then brought to basic conditions with NH4OH and extracted with DCM. The organic phase was dried over Na2SO4 and concentrated in vacuo to dryness to obtain 0.71 g of 1-[4-(4-methyl-piperazin-1-yl-methyl)-phenyl]-ethanone as a yellow oil.

1. temperatureThe resulting suspension was heated
2. temperatureunder reflux for 4 hours
3. temperatureheated
4. temperatureunder reflux for 1 hour
5. customThe two phases were separated
6. washthe aqueous phase rinsed with AcOEt
7. extractionextracted with DCM
8. dry with materialThe organic phase was dried over Na2SO4
9. concentrationconcentrated in vacuo to dryness