反应详情

温度

100 °C

In 3.0 ml of acetic acid was dissolved 1.37 g (5.8 mmol) of 5-nitro-1,10-phenanthroline. A solution prepared by dissolving 1.08 g (4.8 mmol) of stannic chloride (II) dihydrate in 2.2 ml of concentrated hydrochloric acid was added dropwise thereto, followed by stirring at 100° C. for 2 hours. The reaction mixture was made alkaline with a NaOH aqueous solution and extracted with chloroform. After chloroform was distilled off under reduced pressure, a yellow solid was obtained. This was recrystallized from tetrahydrofurane-hexane to obtain 0.75 g (66%) of the desired 5-amino-1,10-phenanthroline (Compound (2)).

1. customA solution prepared
2. additionwas added dropwise
3. extractionextracted with chloroform
4. distillationAfter chloroform was distilled off under reduced pressure
5. customa yellow solid was obtained
6. customThis was recrystallized from tetrahydrofurane-hexane