HRID2179855

反应详情

EQUATION

反应方程式

HRID 2179855 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

Under the nitrogen atmosphere, 9-([2,2′-binaphthalen]-7-yl) anthracene (10.0 g) as the ninth intermediate compound, N-bromosuccinimide (NBS) (4.6 g), iodine (0.1 g), and THF (60 ml) were added to a flask and stirred overnight at room temperature. By adding an aqueous solution of sodium thiosulfate, the reaction was terminated. Liquid separation was performed by adding water and toluene. Subsequently, the solid obtained by distillation of the organic layer under reduced pressure was purified by silica gel column chromatography (solvent: toluene). The solid obtained by distillation of the solvent under reduced pressure was washed with heptane to give 9-([2,2′-binaphthalen]-7-yl)-10-bromoanthracene (11.0 g) as a tenth intermediate compound. The scheme is shown in the following “Reaction 15”.

WORKUP

后处理

  1. customthe reaction was terminated
  2. customLiquid separation
  3. additionby adding water and toluene
  4. customSubsequently, the solid obtained by distillation of the organic layer under reduced pressure
  5. customwas purified by silica gel column chromatography (solvent: toluene)
  6. customThe solid obtained by distillation of the solvent under reduced pressure
  7. washwas washed with heptane