反应详情

温度

130 °C

A mixture of 5-chloro-pyridin-3-ol (1000 mg, 7.72 mmol), potassium tert-butylate (866 mg, 7.72 mmol) and 2-chloro-pyridine (730 g, 7.72 mmol) in DMF (6 mL) was stirred at 130° C. for 3 h. The solvent was removed in vacuo and the residue was partitioned between DCM (50 mL) and 2 N NaOH solution (50 mL). After extraction of the aqueous layer with DCM (6×50 mL) the combined organic layers were dried over MgSO4, filtered, and concentrated in vacuo. The residue was purified by flash chromatography on silica gel (elution with mixtures of hexane and EA) to give the title compound. MS (m/z): 207.2 [M+H+].

1. customThe solvent was removed in vacuo
2. customthe residue was partitioned between DCM (50 mL) and 2 N NaOH solution (50 mL)
3. extractionAfter extraction of the aqueous layer with DCM (6×50 mL) the combined organic layers
4. dry with materialwere dried over MgSO4
5. filtrationfiltered
6. concentrationconcentrated in vacuo
7. customThe residue was purified by flash chromatography on silica gel (elution with mixtures of hexane and EA)