反应详情

A solution of 7-methoxy-3,4,5,6-tetrahydro-2H-azepine (1.0 g, 8.8 mmol) and 3-amino-5-bromopicolinic acid (1.9 g, 8.8 mmol) in DMF (70 mL) was stirred at 130° C. for 48 h. The reaction mixture was diluted with H2O (300 mL) and extracted with DCM (3×300 mL). The combined organic layers were washed with saturated sodium carbonate and brine, dried over Na2SO4. After filtration and concentration, the residue was purified by silica gel chromatography to give the desired product. MS (ESI):294, 296 (MH+).

1. extractionextracted with DCM (3×300 mL)
2. washThe combined organic layers were washed with saturated sodium carbonate and brine
3. dry with materialdried over Na2SO4
4. filtrationAfter filtration and concentration
5. customthe residue was purified by silica gel chromatography