反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
CONDITIONS
反应条件
- 温度
- 85 °C
PROCEDURE
实验过程
Dissolve 4-chloro-1-(4-isopropyl-phenyl)-butan-1-one (5.00 g, 22.2 mmol) and N-bromosuccinimide (4.1 g, 23.0 mmol) in carbon tetrachloride (25 mL) and add AIBN radical initiator (300 mg). Stir and maintain under a nitrogen atmosphere at 80-90° C. or optionally irradiate with a sunlamp until a vigorous exotherm occurs at which point momentarily remove until reflux subsides and then reapply the heat. Reflux for 30 minutes and add another potion of N-bromosuccinimide (100 mg) while maintaining reflux and reflux an additional 15 minutes. Cool to room temperature and precipitate the succinimide from the solution by allowing to stand overnight. Filter and wash the succinimide (2.25 g) with carbon tetrachloride (20 mL). Combine the filtrates and evaporate the solvent in vacuo to give the title compound as a yellow oil (6.80 g, 100%).
WORKUP
后处理
- customoptionally irradiate with a sunlamp until a vigorous exotherm
- custommomentarily remove
- temperatureuntil reflux subsides
- temperatureReflux for 30 minutes
- additionadd another potion of N-bromosuccinimide (100 mg)
- temperaturewhile maintaining
- temperaturereflux
- temperaturereflux an additional 15 minutes
- temperatureCool to room temperature
- customprecipitate the succinimide from the solution
- filtrationFilter
- washwash the succinimide (2.25 g) with carbon tetrachloride (20 mL)
- customCombine the filtrates and evaporate the solvent in vacuo