HRID1296028
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
PROCEDURE
实验过程
After dissolving ethyl 5-bromo-2-ethoxy-4-methylbenzoate (19.72 g) in carbon tetrachloride, azobisisobutyronitrile (1.13 g) was added and the mixture was heated to reflux for 30 minutes. N-bromosuccinimide was added and the mixture was further heated to reflux for 1 hour. The reaction mixture was filtered and the filtrate was concentrated. The residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate) to yield the title compound (10.54 g) as a colorless oil.
WORKUP
后处理
- additionwas added
- temperaturethe mixture was heated
- temperatureto reflux for 30 minutes
- temperaturethe mixture was further heated
- temperatureto reflux for 1 hour
- filtrationThe reaction mixture was filtered
- concentrationthe filtrate was concentrated
- customThe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)