反应详情

To a solution of 5-(5-{5-fluoro-2-(methyloxy)-3-[(E)-2-(methyloxy)ethenyl]phenyl}-1,3,4-thiadiazol-2-yl)-2-(2-methylpropyl)benzonitrile (D36) (130 mg) and sodium iodide (92 mg) in acetonitrile (20 mL) stirred under nitrogen at room temperature was added TMSCl (0.078 mL) dropwise. The reaction mixture was stirred at room temperature for 10 min. Water was added. The aqueous solution was extracted with EA for 3 times. The organic phase was washed with saturated Na2S2O3 solution and saturated brine, dried over sodium sulphate and evaporated in vacuo to afford the crude product 5-{5-[5-fluoro-2-(methyloxy)-3-(2-oxoethyl)phenyl]-1,3,4-thiadiazol-2-yl}-2-(2-methylpropyl)benzonitrile (D37) (75 mg) as a yellow oil. MS (ES): C22H20FN3O2S requires 409. found 410.2 (M+H+).

1. extractionThe aqueous solution was extracted with EA for 3 times
2. washThe organic phase was washed with saturated Na2S2O3 solution and saturated brine
3. dry with materialdried over sodium sulphate
4. customevaporated in vacuo