HRID1266140

反应详情

EQUATION

反应方程式

HRID 1266140 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

1

PROCEDURE

实验过程

A solution of 2,6,7-trichloro-3-pyridin-2-yl-quinoxaline (0.50 g) and 6-dimethylamino-hexylamine (0.46 g) in toluene (25 mL) was refluxed under nitrogen atmosphere for 16 hours. After refluxing, the reaction mixture was cooled, filtered, and concentrated under vacuum. The residue was purified by flash chromatography (silica gel, 1:9 methanol/dichloromethane) to give a yellow solid. Recrystallization from methanol and water gave the product as a fluffy yellow powder (0.41 g); mp 88-90° C.

WORKUP

后处理

  1. temperatureAfter refluxing
  2. temperaturethe reaction mixture was cooled
  3. filtrationfiltered
  4. concentrationconcentrated under vacuum
  5. customThe residue was purified by flash chromatography (silica gel, 1:9 methanol/dichloromethane)
  6. customto give a yellow solid
  7. customRecrystallization from methanol and water