HRID1296028

反应详情

EQUATION

反应方程式

HRID 1296028 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

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

  1. additionwas added
  2. temperaturethe mixture was heated
  3. temperatureto reflux for 30 minutes
  4. temperaturethe mixture was further heated
  5. temperatureto reflux for 1 hour
  6. filtrationThe reaction mixture was filtered
  7. concentrationthe filtrate was concentrated
  8. customThe residue was purified by silica gel column chromatography (solvent: n-hexane-ethyl acetate)