反应详情

To a flask were added 1.06 g of di-(2-picolyl)amine and 20 ml of acetonitrile. The solution was stirred under nitrogen, when 0.7 g of triethylamine were added, followed by 1.5 g of trimethylacetyl chloride. After 1 hour, 20 ml of water were added and the acetonitrile was removed. The product was extracted with ethyl acetate and washed with water. Following solvent removal, the product was recrystallized by dissolving in 6 ml hot hexane with 0.5 ml 2-propanol. Another 2 ml hexane were added and the mixture was cooled to 5 C, filtered, washed with hexane and dried, resulting in 1.3 g of an off-white solid.

1. customthe acetonitrile was removed
2. extractionThe product was extracted with ethyl acetate
3. washwashed with water
4. customFollowing solvent removal
5. customthe product was recrystallized
6. dissolutionby dissolving in 6 ml hot hexane with 0.5 ml 2-propanol
7. additionAnother 2 ml hexane were added
8. temperaturethe mixture was cooled to 5 C
9. filtrationfiltered
10. washwashed with hexane
11. customdried