反应详情

Methanesulphonyl chloride (1.16 mmol) was added to a stirred solution of Intermediate 125 (0.033 mmol) and pyridine (0.5 ml) in chloroform (1 ml) at room temperature. After stirring at room temperature for 31 h, the reaction mixture was applied to a SPE cartridge (aminopropyl, 5 g) and the cartridge was eluted sequentially with chloroform, ethyl acetate and methanol. Fractions containing the desired product were evaporated in vacuo. The resulting residue was further purified on a SPE cartridge (silica, 1 g) eluting with a gradient of 30-100% ethyl acetate in petroleum ether to afford Example 176. LCMS showed MH+=490, TRET=2.97 min.

1. washthe cartridge was eluted sequentially with chloroform, ethyl acetate and methanol
2. additionFractions containing the desired product
3. customwere evaporated in vacuo
4. customThe resulting residue was further purified on a SPE cartridge (silica, 1 g)
5. washeluting with a gradient of 30-100% ethyl acetate in petroleum ether
6. customto afford Example 176
7. customMH+=490, TRET=2.97 min.