反应详情

温度

-70 °C

To a 125 mL 3N round-bottomed flask equipped with N2 inlet and septum were added 3.59 g (15.7 mmol) 3-isopropoxy-4-bromotoluene and 30 mL dry tetrahydrofuran. The solution was cooled to −70° C. and 7.5 mL (18.8 mmol) of a 2.5 M solution of butyl lithium in hexane was added over 5 minutes, and the solution stirred 5 minutes at −70° C. Then 3.2 mL (18.8 mmol) triethyl borate was added, followed by stirring for 5 minutes at −70° C. and then stirring at room temperature for 24 hours. The reaction was quenched with 1 N aqueous hydrochloric acid and extracted into ethyl acetate. The organic layer was washed with water and brine, dried over sodium sulfate, and evaporated. The residue was triturated with hexane to a white solid, 1.7 g (56%).

1. customTo a 125 mL 3N round-bottomed flask equipped with N2 inlet
2. stirringby stirring for 5 minutes at −70° C.
3. stirringstirring at room temperature for 24 hours
4. customThe reaction was quenched with 1 N aqueous hydrochloric acid
5. extractionextracted into ethyl acetate
6. washThe organic layer was washed with water and brine
7. dry with materialdried over sodium sulfate
8. customevaporated
9. customThe residue was triturated with hexane to a white solid, 1.7 g (56%)