反应详情

温度

90 °C

In 130 ml of carbon tetrachloride was dissolved 10 g of ethyl 2-methylbiphenyl-4-carboxylate, the whole was heated to 90° C. and then 1.0 g of NBS and 136 mg of 2,2′-azobisisobutyronitrile were added thereto. After the reaction solution was heated under reflux, 6.78 g of NBS was added thereto and the whole was heated under reflux for 1 hour and a half. After the reaction solution was cooled to room temperature, precipitate was removed by filtration, water was added to the filtrate, and the organic layer was extracted with carbon tetrachloride. After the resulting organic layer was dried over anhydrous magnesium sulfate, the solvent was removed by evaporation to obtain 13.6 g of ethyl 2-(bromomethyl)biphenyl-4-carboxylate as a white solid.

1. temperatureAfter the reaction solution was heated
2. temperatureunder reflux
3. temperaturethe whole was heated
4. temperatureunder reflux for 1 hour
5. temperatureAfter the reaction solution was cooled to room temperature
6. customprecipitate was removed by filtration, water
7. additionwas added to the filtrate
8. extractionthe organic layer was extracted with carbon tetrachloride
9. dry with materialAfter the resulting organic layer was dried over anhydrous magnesium sulfate
10. customthe solvent was removed by evaporation