反应详情

A solution of 5-(4-fluorophenyl)-thieno[3,2-b]pyridin-7-ol (1.6 g) in phosphorus oxychloride (50 mL) is refluxed for 3 hours. After the excess phosphorus oxychloride is removed under vacuum, the residue is treated with ethyl acetate (20 mL), and NaOH (2N, 20 mL). The mixture is extracted with ethyl acetate (3×20 mL) and the combined organic layers are washed with brine and dried over MgSO4. Evaporation of the solvent gives 7-chloro-5-(4-fluorophenyl)thieno[3,2-b]pyridine (1.5 g, 88% yield) as a white solid, m.p. 119-121° C.

1. customAfter the excess phosphorus oxychloride is removed under vacuum
2. additionthe residue is treated with ethyl acetate (20 mL), and NaOH (2N, 20 mL)
3. extractionThe mixture is extracted with ethyl acetate (3×20 mL)
4. washthe combined organic layers are washed with brine
5. dry with materialdried over MgSO4
6. customEvaporation of the solvent