HRID1456827

反应详情

EQUATION

反应方程式

HRID 1456827 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

To a solution of 2-(4-methylsulfonylphenyl)-1-phenylazulene (0.43 g) in CCl4 (20.0 ml) was added N-bromosuccinimide (0.23 g) and α,α'-azobis(isobutyronitrile) (0.01 g), and the reaction mixture was heated under reflux for 1 hr. The mixture was cooled to room temperature and was filtered, and concentrated. The crude product was purified by SiO2 column chromatography (benzene/EtOAc, 20:1) to give the title compound (0.52 g) as green crystals; mp 172°-173° C.

WORKUP

后处理

  1. temperaturethe reaction mixture was heated
  2. temperatureunder reflux for 1 hr
  3. filtrationwas filtered
  4. concentrationconcentrated
  5. customThe crude product was purified by SiO2 column chromatography (benzene/EtOAc, 20:1)