反应详情

温度

100 °C

Sodium ethanethiol (0.108 g, 1.29 mmol) was added to a solution of 2-(2-oxo-2H-pyridin-1-yl)-anisole (0.100 g, 0.497 mmol) in DMF (2 mL), and the reaction mixture was heated at 100° C. for 3 hr. The reaction mixture was partitioned between CHCl3 and saturated aqueous ammonium chloride and treated with 8N HCl (pH=1). The organic layer was separated, washed with H2O, brine, dried (Na2SO4), filtered, concentrated, and taken up in EtOAc, then extracted with 2% NaOH solution. The aqueous basic layer was acidified with 10% HCl solution, then extracted with EtOAc, the organic layer washed with brine, dried (Na2SO4), filtered, and concentrated to give the desired product.

1. customThe reaction mixture was partitioned between CHCl3 and saturated aqueous ammonium chloride
2. additiontreated with 8N HCl (pH=1)
3. customThe organic layer was separated
4. washwashed with H2O, brine
5. dry with materialdried (Na2SO4)
6. filtrationfiltered
7. concentrationconcentrated
8. extractionextracted with 2% NaOH solution
9. extractionextracted with EtOAc
10. washthe organic layer washed with brine
11. dry with materialdried (Na2SO4)
12. filtrationfiltered
13. concentrationconcentrated