反应详情

A mixture of 2-(4-(3-(4-chlorophenyl)-1,2,4-thiadiazol-5-yl)piperazin-1-yl)-1-(4-methoxyphenyl)ethanol (30 mg, 69.6 μmol) and DAST (22.4 mg, 18.4 μl, 139 μmol) in 2 mL DCM at 0-5° C. was warmed to RT and stirred for 2 h. 10% aq. Na2CO3-solution was added and stirred for 10 min. The organic layer was separated and concentrated in vacuo. The residue was purified by column chromatography on silica eluting with a gradient formed from heptane and EtOAc to yield, after evaporation of the product containing fraction, 24 mg (80%) of the title compound as light yellow solid. MS (m/e): 433.3 (MH+).

1. stirringstirred for 10 min
2. customThe organic layer was separated
3. concentrationconcentrated in vacuo
4. customThe residue was purified by column chromatography on silica eluting with a gradient
5. customformed from heptane and EtOAc
6. customto yield
7. customafter evaporation of the product
8. additioncontaining fraction, 24 mg (80%) of the title compound as light yellow solid