HRID2258508

反应详情

EQUATION

反应方程式

HRID 2258508 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

To a cooled suspension of 7-chloro-2-(5-hydroxybenzofuran-2-yl)quinoline (0.71 g) in tetrahydrofuran (12 ml), sodium hydride (60% in mineral oil, 0.125 g) was added below 10° c. After being stirred for 15 minutes, α,α'-dichloro-o-xylene (1.68 g) was added to the mixture. After subsequently being stirred at ambient temperature for 1.5 hours, the mixture was refluxed for 25 hours. After the solvent was removed under reduced pressure, the residue was subjected to column chromatography on silica gel (25 g) and eluted with a mixture of chloroform and n-hexane (1:1). The fractions containing object compound were combined and concentrated under reduced pressure give 7-chloro-2-[5-(2-chloromethylbenzyloxy)benzofuran-2-yl]quinoline (0.56 g).

WORKUP

后处理

  1. additionwas added below 10° c
  2. stirringAfter subsequently being stirred at ambient temperature for 1.5 hours
  3. temperaturethe mixture was refluxed for 25 hours
  4. customAfter the solvent was removed under reduced pressure
  5. washeluted with a mixture of chloroform and n-hexane (1:1)
  6. additionThe fractions containing object compound
  7. concentrationconcentrated under reduced pressure