HRID619743

反应详情

EQUATION

反应方程式

HRID 619743 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

CONDITIONS

反应条件

温度
80 °C

PROCEDURE

实验过程

4-(5-Isoquinolylsulfanyl)-1,2-benzenediamine 200 mg (0.7 mmol) was dissolved in water 10 ml, a water solution 6 ml of glyoxal-sodium bisulfite hydrate 580 mg (2.3 mmol) was added, and the mixture was stirred for 1 hour at 80° C. Potassium carbonate was added to the reaction solution to alkalize the solution, and the solution was extracted with ethyl acetate. The organic layer was washed with saturated sodium chloride, and concentrated under reduced pressure. The resulting residue was purified by silica gel column chromatography (chloroform:acetone=1:10), and 6-(5-isoquinolylsulfanyl)quinoxaline 90 mg (41.2%) was obtained.

WORKUP

后处理

  1. extractionthe solution was extracted with ethyl acetate
  2. washThe organic layer was washed with saturated sodium chloride
  3. concentrationconcentrated under reduced pressure
  4. customThe resulting residue was purified by silica gel column chromatography (chloroform:acetone=1:10)