反应详情

温度

60 °C

To a solution of (3-(4-chloro-2-methoxyphenyl)-1,2,4-thiadiazol-5-yl)methanol (0.08 g, 0.31 mmol) in toluene (4 ml) was added PBr3 (49 μl, 0.47 mmol) and the resulting reaction mixture was heated at 60° C. for 2 h. After the completion of the reaction (TLC monitoring), the reaction mixture was cooled to 0° C., added water (50 ml) and extracted with ethyl acetate (3×50 ml). The combined organics was washed with saturated NaHCO3 solution, dried over Na2SO4, filtered and concentrated under vacuum. The crude residue was purified over silica gel (100-200 M, 5% EtOAc-Hexane) to get the desired product (0.063 g, 64%). MS: 319 (M+H)+.

1. customthe resulting reaction mixture
2. customAfter the completion of the reaction (TLC monitoring)
3. temperaturethe reaction mixture was cooled to 0° C.
4. extractionextracted with ethyl acetate (3×50 ml)
5. washThe combined organics was washed with saturated NaHCO3 solution
6. dry with materialdried over Na2SO4
7. filtrationfiltered
8. concentrationconcentrated under vacuum
9. customThe crude residue was purified over silica gel (100-200 M, 5% EtOAc-Hexane)