反应详情

To a solution of 5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-3-{2-methyl-3-[(E)-2-(methyloxy)ethenyl]phenyl}-1,2,4-thiadiazole (D105) (130 mg, 0.324 mmol) and sodium iodide (97 mg, 0.649 mmol) in Acetonitrile (8 mL) stirred under nitrogen at room temperature was added TMSCl (0.083 mL, 0.649 mmol) dropwise. The reaction mixture was stirred at room temperature for 1 hr. Water was added. The aqeuous 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 [3-(5-{3-chloro-4-[(1-methylethyl)oxy]phenyl}-1,2,4-thiadiazol-3-yl)-2-methylphenyl]acetaldehyde (D106) (120 mg) as a yellow oil, which was used for the next step without further purification. MS (ES): C20H19ClN2O2S requires 386.1. found 387.2 (M+H+).

1. extractionThe aqeuous 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