反应详情

温度

0 °C

Methane sulfonyl chloride (7.87 μl, 0.101 mmol) was added to a mixture of 3-chloro-N-{2-(3-hydroxy-1-propyn-1-yl)-6-methyl-3-[3-(methyloxy)phenyl]thieno[2,3-b]pyridin-4-yl}benzenesulfonamide (Example 85) (42 mg, 0.084 mmol) and Hunig's base (17.64 μl, 0.101 mmol) in THF (395 μl) and the mixture stirred at 0° C. The mixture was slowly allowed to warm to RT, with stirring, for 2 h. The mixture was then evaporated to dryness and the residue purified on silica, eluting with a gradient of 0-100% ethyl acetate in cyclohexane, to afford the title compound (14 mg). LCMS (A) m/z: 517 [M+1]+ (displacement of OSO2Me by methanol), Rt 1.45 min (acidic).

1. temperatureto warm to RT
2. stirringwith stirring, for 2 h
3. customThe mixture was then evaporated to dryness
4. customthe residue purified on silica
5. washeluting with a gradient of 0-100% ethyl acetate in cyclohexane