反应详情

温度

120 °C

To a suspension of 5-(5-bromo-1,3,4-thiadiazol-2-yl)-2-(2-methylpropyl)benzonitrile (D26) (151 mg), 2-{2-ethyl-3-[(E)-2-(methyloxy)ethenyl]phenyl}-4,4,5,5-tetramethyl-1,3,2-dioxaborolane (203 mg) and tripotassium phosphate (249 mg) in N,N-dimethylformamide (DMF) (6 mL) and water (1.5 mL) under nitrogen was added Pd(Ph3P)4 (54.2 mg). The reaction vessel was sealed and heated under microwave at 120° C. for 10 min. Water was added. The reaction mixture was extracted with EA for 3 times, the combined organic layers were washed with brine, dried over anhydrous sodium sulfate, the dried solution was concentrated, and purified by column chromatography to afford 5-(5-{2-ethyl-3-[(E)-2-(methyloxy)ethenyl]phenyl}-1,3,4-thiadiazol-2-yl)-2-(2-methylpropyl)benzonitrile (D30) (185 mg) as a yellow oil. MS (ES): C24H25N3OS requires 403. found 404.2 (M+H+).

1. customThe reaction vessel was sealed
2. extractionThe reaction mixture was extracted with EA for 3 times
3. washthe combined organic layers were washed with brine
4. dry with materialdried over anhydrous sodium sulfate
5. concentrationthe dried solution was concentrated
6. custompurified by column chromatography