反应详情

温度

0 °C

Diphenyl ether (0.85 g) was dissolved in anhydrous tetrahydrofuran (20 ml) and the reaction mixture was cooled to 0° C. N-butyllithium (1.6M, 3.1 ml) was delivered by drops thereto and the reaction mixture was stirred for 30 minutes at the same temperature. Trimethyl borate (0.68 ml) was added thereto and the reaction mixture was stirred for two hours at room temperature. 1N hydrochloric acid was added to the reaction mixture and the water layer was extracted with ethyl acetate. The organic layer was dried with anhydrous sodium sulfate. The solvent was distilled off and the obtained residue was purified by column chromatography (ethyl acetate:hexane=1.5:1 to 1:3) to obtain the title compound (304 mg) having the following physical data.

1. stirringthe reaction mixture was stirred for two hours at room temperature
2. extractionthe water layer was extracted with ethyl acetate
3. dry with materialThe organic layer was dried with anhydrous sodium sulfate
4. distillationThe solvent was distilled off
5. customthe obtained residue was purified by column chromatography (ethyl acetate:hexane=1.5:1 to 1:3)