HRID1354533

反应详情

EQUATION

反应方程式

HRID 1354533 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

2

PROCEDURE

实验过程

5-Amino-1,10-phenanthroline (350 mg, 1.8 mmol) was refluxed with glutaric anhydride (2.0g, 17.5 mmol) in pyridine (3 mL) and triethylamine (3 mL) for 2 hours. The reaction mixture was reduced to a viscous oil by rotary evaporation. Column purification on silica with 10% methanol in methylene chloride (product produced bright red spots with Fe(II) on TLC) gave the crude product (320 mg 1.1 mmol). Further purification of the crude product was by recrystallization once from 30 mL boiling water to give the title compound (250 mg, 0.85 mmol) as centimeter long transparent needles.

WORKUP

后处理

  1. customThe reaction mixture was reduced to a viscous oil by rotary evaporation
  2. customColumn purification on silica with 10% methanol in methylene chloride (product produced bright red spots with Fe(II) on TLC)
  3. customgave the crude product (320 mg 1.1 mmol)
  4. customFurther purification of the crude product
  5. customwas by recrystallization once from 30 mL