反应详情

To a solution of 3-bromo-2,6-dimethylthieno[2,3-b]pyridin-4-amine (1.6 g, 6.22 mmol) (Description 8) in THF (30 mL) was added potassium tert-butoxide (2.79 g, 24.89 mmol) and the mixture stirred for 5 min before adding 3-chlorobenzenesulfonyl chloride (2.190 mL, 15.56 mmol). The mixture was stirred for 1 h and the solvent was then removed in vacuo. Ethyl acetate (50 mL) was added and the mixture washed with water (3×30 mL). The organic layer was dried over MgSO4, filtered and the solvent removed in vacuo. Purification by chromatography on silica gel, eluting with a gradient of 0-30% ethyl acetate in cyclohexane, afforded the title compound (1.3 g). LCMS (A) m/z: 431/433 [M+1]+, Rt 1.38 min (acidic).

1. stirringThe mixture was stirred for 1 h
2. customthe solvent was then removed in vacuo
3. additionEthyl acetate (50 mL) was added
4. washthe mixture washed with water (3×30 mL)
5. dry with materialThe organic layer was dried over MgSO4
6. filtrationfiltered
7. customthe solvent removed in vacuo
8. customPurification by chromatography on silica gel
9. washeluting with a gradient of 0-30% ethyl acetate in cyclohexane