HRID554575

反应详情

EQUATION

反应方程式

HRID 554575 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 1-(4-ethylbenzyl)-1H-indole (2.0 g, 8.50 mmol) in DMF (20 mL) was added dropwise to a solution of bromine (0.46 mL, 8.93 mmol) in DMF (20 mL) at room temperature. The reaction mixture was stirred for two hours, and then poured into an ice-cooled sodium pyrosulfurous acid aqueous solution. The resulting mixture was extracted with ethyl acetate, and the organic layer was washed with a saturated sodium hydrogencarbonate aqueous solution and a saturated sodium chloride aqueous solution and dried (anhydrous magnesium sulfate), and then the solvent was distilled under reduced pressure. The residue was recrystallized from ethyl acetate and n-hexane to obtain the title compound (1.68 g, 63%).

WORKUP

后处理

  1. extractionThe resulting mixture was extracted with ethyl acetate
  2. washthe organic layer was washed with a saturated sodium hydrogencarbonate aqueous solution
  3. dry with materiala saturated sodium chloride aqueous solution and dried (anhydrous magnesium sulfate)
  4. distillationthe solvent was distilled under reduced pressure
  5. customThe residue was recrystallized from ethyl acetate and n-hexane