Related Products of 24100-18-3, Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps,and cheap raw materials. 24100-18-3, name is 2-Bromo-3-methoxypyridine. A new synthetic method of this compound is introduced below.
Step A 2-Bromo-3-methoxy-6-nitropyridine To a 500 mL round bottomed flask fitted with a Teflon stir bar and a thermometer was added 90 mL of concentrated sulphuric acid and 37.6 g of 2-bromo-3-methoxypyridine (200 mmol). The flask was warmed in an oil bath to 60 C. Added slowly over 1h 16.5 mL (350 mmol) of fuming nitric acid (90%, d=1.50). Maintain the temperature between 60 and 70 during the addition. Stir at 60 for 3h after the addition was complete, then at room temperature overnight. By TLC (70/30 hex/EtOAc) is consumed. The product mixture was poured into 600 mL of ice/water, from which the product precipitated. This material was filtered, washed with 3*200 mL of cold water and then 100 mL of saturated sodium bicarbonate. After drying in the filter funnel in a stream of air, the remaining water was removed under reduced pressure, to give 16.5 g of a solid. H NMR (400 MHz, CDCl3): delta 8.27(d, J=8 Hz,1H); 6.32(d, J=8 Hz,1H); 4.06(s, 3H).
At the same time, in my other blogs, there are other synthetic methods of this type of compound,24100-18-3, 2-Bromo-3-methoxypyridine, and friends who are interested can also refer to it.
Reference:
Patent; Merck & Co., Inc.; US5929094; (1999); A;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem