反应详情

A solution of 2,6-dichloropyridin-4-amine 41.6.A (available from Aldrich) (3.10 g, 19.0 mmol) in 20% NaOMe/MeOH (15 mL) was refluxed for 72 hr. The reaction mixture was diluted with H2O (40 mL) and extracted with 30% iPrOH/CHCl3 (3×30 mL). The combined organic layers were washed with water (2×20 mL), brine (15 mL) and dried over MgSO4. After removal of organic solvents under reduced pressure, purification of the residue by flash chromatography on silica gel using 0-10% MeOH/CH2Cl2 for elution gave title product 41.6.B as white solid (2.45 g, 81.2%).

1. extractionextracted with 30% iPrOH/CHCl3 (3×30 mL)
2. washThe combined organic layers were washed with water (2×20 mL), brine (15 mL)
3. dry with materialdried over MgSO4
4. customAfter removal of organic solvents
5. customunder reduced pressure, purification of the residue by flash chromatography on silica gel using 0-10% MeOH/CH2Cl2
6. washfor elution