反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
0.15 g (0.519 mmol) of 2-acetylamino-4-(6-nitropyridin-3-yl)-1H-pyrrole-3-carboxamide is added at a temperature in the region of 25° C. to a suspension of 0.015 g (0.014 mmol) of 10% palladium on carbon in 20 cm3 of methanol. After hydrogenating for 2 hours in an autoclave under 2 bar of hydrogen, at a temperature in the region of 30° C., the reaction mixture is filtered, the catalyst is rinsed with twice 2 cm3 of ethyl ether. After draining and drying, 0.11 g of 2-acetylamino-4-(6-aminopyridin-3-yl)-1H-pyrrole-3-carboxamide is obtained, in the form of a brown solid. 1H NMR (400 MHz, (CD3)2SO, —δ in ppm) 2.13 (s, 3H); 6.01 (broad s, 2H); from 5.50 to 8.85 (very broad m, 2H); 6.35 (d, J=2.5 Hz, 1H); 6.49 (d, J=8.5 Hz, 1H); 7.36 (dd, J=2.5 and 8.5 Hz, 1H); 7.87 (d, J=2.5 Hz, 1H); 10.65 (s, 1H); 11.35 (broad s, 1H).
WORKUP
后处理
- filtrationthe reaction mixture is filtered
- washthe catalyst is rinsed with twice 2 cm3 of ethyl ether
- customdrying