反应详情

To a flask were added 2.0 g of 2,2′-dipyridylamine and 35 ml of acetonitrile. The solution was stirred under nitrogen and cooled to 5 C, when 1.5 g of triethylamine were added, followed by 1.5 g of trimethylacetyl chloride and the mixture was allowed to warm to 22 C. After 1 hour, 50 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 purified by silica gel chromatography using 50% ethyl acetate in hexane, resulting in 1.8 g of an oil that solidified on standing.

1. additionwere added
2. temperatureto warm to 22 C
3. customthe acetonitrile was removed
4. extractionThe product was extracted with ethyl acetate
5. washwashed with water
6. customFollowing solvent removal
7. customthe product was purified by silica gel chromatography