反应详情

2-Chloro-3-bromopyridine (0.25 g, 1.3 mmol), D2 (0.25 g, 1.3 mmol) and potassium carbonate (0.23 g, 2.9 mmol) in DMF (5 ml) were heated at 120° C. for 16 h. The mixture was concentrated and the residue partitioned between EtOAc and water (50 ml each). The aqueous was re-extracted with EtOAc (50 ml) and the combined organics washed with water, dried (Na2SO4) and concentrated. Purification by column chromatography on silica (0-50% diethyl ether\40-60 pet. ether gradient) gave the title compound as a yellow solid (0.26 g). δH (CDCl3) 1.64 (2H, m), 2.17 (2H, d), 2.98 (2H, m), 3.43 (2H, m), 3.74 (2H, m), 6.58 (2H, m), 6.77 (1H, m), 6.89 (2H, m), 7.78 (1H, d), 8.22 (1H, dd). MS (ES): MH+ 351.

1. concentrationThe mixture was concentrated
2. customthe residue partitioned between EtOAc and water (50 ml each)
3. extractionThe aqueous was re-extracted with EtOAc (50 ml)
4. washthe combined organics washed with water
5. dry with materialdried (Na2SO4)
6. concentrationconcentrated
7. customPurification by column chromatography on silica (0-50% diethyl ether\40-60 pet. ether gradient)