反应详情

To a flask were added 5.2 g pulverized potassium hydroxide and 35 ml dimethylsulfoxide. After adding 3.4 g 2,2′-dipyridylamine, the mixture was stirred under nitrogen for 45 minutes, when 3.3 g 2-(chloromethyl)pyridine hydrochloride was added. After stirring for 1 hour, 100 ml of water was added and the product was extracted with 60 ml of 50% ethyl acetate, 50% hexane. The organic layer was washed with 30 ml water and the solvent was removed. The residue was added to 5 ml hot ethanol, and 20 ml of water was added. After cooling to 5 C, the solid was filtered and washed with water. The product was dissolved in 20 ml hot ethanol and treated with 150 mg activated carbon. After hot filtration through celite, 40 ml of water were added and the mixture was cooled to 5 C. The product was filtered, washed with 20 ml 20% ethanol in water, and dried resulting in 2.9 g of an off-white solid.

1. additionTo a flask were added 5.2 g
2. stirringAfter stirring for 1 hour
3. extractionthe product was extracted with 60 ml of 50% ethyl acetate, 50% hexane
4. washThe organic layer was washed with 30 ml water
5. customthe solvent was removed
6. additionThe residue was added to 5 ml hot ethanol, and 20 ml of water
7. additionwas added
8. temperatureAfter cooling to 5 C
9. filtrationthe solid was filtered
10. washwashed with water
11. dissolutionThe product was dissolved in 20 ml hot ethanol
12. additiontreated with 150 mg
13. filtrationAfter hot filtration through celite, 40 ml of water
14. additionwere added
15. temperaturethe mixture was cooled to 5 C
16. filtrationThe product was filtered
17. washwashed with 20 ml 20% ethanol in water
18. customdried