反应详情

温度

100 °C

To a solution of (3-(2-(benzyloxy)-4-chlorophenyl)-1,2,4-thiadiazol-5-yl) methanol (0.35 g, 1.05 mmol) in toluene (10 ml) was added PBr3 (0.16 ml, 1.58 mmol) and the resulting reaction mixture was heated at 100° C. for 15 min. 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 to get the desired product (0.33 g, 79% crude yield), that was carried forward as such for the next step. MS: 395.05 (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