反应详情

To the solution of LiHMDS (5.18 g, 0.026 mmol, 1.3 equiv.) was added picolinonitrile (2.08 g, 0.02 mmol, 1 equiv.) at ice-bath and kept stirred for 2 h. Then, the reaction mixture was acidified with aqueous HCl (4N) to pH2, cooled at ice-bath and kept stirred. Then, the mixture was extracted with EA (200 mL×5). The combined organic phase was washed with brine, dried (Na2SO4), and evaporated to get picolinimidamide (2.0 g, 83%). LC-MS (m/z)=122 [M+H]+.

1. temperaturecooled at ice-bath
2. stirringkept stirred
3. extractionThen, the mixture was extracted with EA (200 mL×5)
4. washThe combined organic phase was washed with brine
5. dry with materialdried (Na2SO4)
6. customevaporated