反应详情

温度

50 °C

Dissolve 2-bromo-1-[6-(difluoromethyl)-3-pyridyl]propan-1-one (0.500 g, 1.89 mmol) and acetyl guanidine (0.514 g, 5.68 mmol) in DMF (12 mL). Heat the mixture to 50° C., and stir for 16 hours. Pour the mixture into water, and extract with EtOAc (3×20 mL). Dry the combined organic extracts over sodium sulfate; filter; collect the filtrate; and concentrate the filtrate under reduced pressure. Purify the resulting residue by flash chromatography (silca gel) eluting with a 40:1 ratio of DCM/MeOH to give the title compound as a white solid (0.229 g, 46% yield). LCMS (m/z) 267 (M+1).

1. extractionextract with EtOAc (3×20 mL)
2. dry with materialDry the combined organic extracts over sodium sulfate
3. filtrationfilter
4. customcollect the filtrate
5. concentrationand concentrate the filtrate under reduced pressure
6. customPurify the resulting residue by flash chromatography (silca gel)
7. washeluting with a 40:1 ratio of DCM/MeOH