反应详情

Isovaleryl chloride (0.04 mmol) was added to a stirred solution of Intermediate 125 (0.033 mmol) and diisopropylethylamine (0.1 mmol) in chloroform (1 ml) at room temperature. After stirring at room temperature for 1.5 h, the reaction mixture was applied to a SPE cartridge (aminopropyl, 1 g) and the cartridge was eluted sequentially with chloroform, ethyl acetate and methanol. Fractions containing the desired product were combined and blown down under nitrogen. 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+=496, TRET=3.17 min.

1. washthe cartridge was eluted sequentially with chloroform, ethyl acetate and methanol
2. additionFractions containing the desired product
3. customThe resulting residue was further purified on a SPE cartridge (silica, 1 g)
4. washeluting with a gradient of 30-100% ethyl acetate in petroleum ether
5. customto afford Example 176
6. customMH+=496, TRET=3.17 min.