Electric Literature of 39856-50-3 ,Some common heterocyclic compound, 39856-50-3, molecular formula is C5H3BrN2O2, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc., below Introduce a new synthetic route.
Under a nitrogen purge, the solid 4-bromo-2-nitropyridine (10. Ig; 0.05mol), potassium carbonate (10.5g; 0.075mol; -325mesh), tetrabutylammonium iodide (1.25g; 5mol%), and piperazine (5.4g; 0.0625mol) were sequentially added to 80ml acetonitrile. The suspension was heated to reflux, and maintained for 16 h. The now-bright yellow suspension was filtered hot, and the filter cake washed with a few portions of hot acetonitrile, such that the filtrate flows only slightly yellow. The filtrate quickly deposited a yellow/orange solid. This was reheated to obtain a clear solution, which was placed in the refrigerator for 16 h. The yellow/orange solid was isolated by filtration and the filter cake was washed with small portion cold CH3CN, followed by a small portion of petroleum ether. Air drying the solid provided ca 10.2g of solid material, about 65% of theory. Another 2g of material was isolated by evaporating the acetonitrile filtrate down to a semi-solid and then recrystallizing the residue from a minimum amount of hot isopropanol (treated with activated charcoal). NMR: 1.63 (s, IH), 2.99 (m, 4H), 3.36 (m, 4H), 7.14 (m, IH), 8.08 (m, 2H), m/z 209.
In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles. 39856-50-3, 5-Bromo-2-nitropyridine, other downstream synthetic routes, hurry up and to see.
Reference:
Patent; ASTRAZENECA AB; ASTRAZENECA UK LIMITED; WO2006/95159; (2006); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem