反应详情

温度

0 °C

4-(3-Chloro-4-fluorophenyl)-3-[4-(hydroxymethyl)-1,2,5-oxadiazol-3-yl]-1,2,4-oxadiazol-5(4H)-one (250 mg, 0.7996 mmol) was dissolved in anhydrous DCM (8 mL) followed by addition of triethylamine (TEA) (134 μL, 0.96 mmol). Reaction was cooled to 0° C. and methanesulfonyl chloride (68 μL, 0.88 mmol) was added dropwise. The reaction was diluted with water and extracted with ethyl acetate three times, dried with sodium sulfate, filtered, and concentrated in vacuo. The crude residue was purified by flash column chromatography eluting with 25%-70% EtOAc to yield the desired product (259 mg, 83%). MF=C12H8ClFN4O6S; LCMS calculated for C12H9ClFN4O6S (M+H)+: m/z=390.992.

1. customReaction
2. extractionextracted with ethyl acetate three times
3. dry with materialdried with sodium sulfate
4. filtrationfiltered
5. concentrationconcentrated in vacuo
6. customThe crude residue was purified by flash column chromatography
7. washeluting with 25%-70% EtOAc