HRID1354533
反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
产物
AUXILIARIES
试剂、催化剂与溶剂
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
- customThe reaction mixture was reduced to a viscous oil by rotary evaporation
- customColumn purification on silica with 10% methanol in methylene chloride (product produced bright red spots with Fe(II) on TLC)
- customgave the crude product (320 mg 1.1 mmol)
- customFurther purification of the crude product
- customwas by recrystallization once from 30 mL