反应详情

According to Scheme 5 Step 5 Method B: A suspension of (bromomethyl)benzene (0.61 mmol, 74 μL), N-(3-chloro-4-(piperazin-1-yl)phenyl)picolinamide (0.51 mmol, 161 mg) and of K2CO3 (0.51 mmol, 70 mg) in ACN (3 mL) was stirred at 80° C. for 30 minutes. After evaporation of the solvent, water and AcOEt were added. The aqueous phase was extracted with AcOEt. The organic phase was washed with brine, was dried over Na2SO4, was filtered and was concentrated under reduced pressure. The crude product was purified by flash chromatography over silica gel using DCM/AcOEt (80:20) as eluent and finally crystallized in pentane to obtain N-(4-(4-benzylpiperazin-1-yl)-3-chlorophenyl)picolinamide (0.98 mmol, 40 mg, 20%) as a white solid.

1. customAfter evaporation of the solvent, water and AcOEt
2. additionwere added
3. extractionThe aqueous phase was extracted with AcOEt
4. washThe organic phase was washed with brine
5. dry with materialwas dried over Na2SO4
6. filtrationwas filtered
7. concentrationwas concentrated under reduced pressure
8. customThe crude product was purified by flash chromatography over silica gel
9. customfinally crystallized in pentane