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. 6419-36-9, name is 2-(Pyridin-3-yl)acetic acid hydrochloride. A new synthetic method of this compound is introduced below., 6419-36-9
Example C2 Synthesis of 3-pyridyl-1-hydroxyethylidene-1,1-bisphosphonic Acid In a 100 ml rounded bottom, three necked flask equipped with a magnetic stirrer, a thermometer, a reflux condenser and a compensated-pressure dropping funnel were charged: 1.00 g (5.76¡¤10-3 mol) of 3-pyridyl acetic acid hydrochloride, 1.46 g (1.78¡¤10-2 mol) of phosphonic acid, 3.01 g (1.72¡¤10-2 mol) of methanesulfonic anhydride and 7.2 ml of toluene. 1.22 g of PCl5 was steeply added at room temperature. Exothermy, gas evolution and foaming was observed. The mixture was then heated up to 95 C. At about 40 C., formation of two well defined liquid phases were observed. The mixture was kept overnight at 95 C. No stirring problems arose. The mixture was then let to cool down to 80 C. at which point 7.2 ml of water were added dropwise (exothermy was observed). The mixture was stirred at 80 C. for 15 minutes and then let to cool down to room temperature. The aqueous layer was decanted and heated to 95 C. for 5.5 h and let to cool down to room temperature, at which point 7.2 ml of ethanol were added. The resulting mixture was cooled down to 5 C., stirred for 1 h and filtered. The solid washed with ethanol and dried at 40 C. in a vacuum oven until constant weight. 1.01 g of 3-pyridyl-1-hydroxyethylidene-1,1-bisphosphonic acid monohydrate are obtained (Yield: 58.23%) Chromatographic purity: 98.327% (area percent)
At the same time, in my other blogs, there are other synthetic methods of this type of compound,6419-36-9, 2-(Pyridin-3-yl)acetic acid hydrochloride, and friends who are interested can also refer to it.
Reference:
Patent; Serrano, Jordi Puig; Illado, Jordi Bosch; US2008/194525; (2008); A1;,
Pyridine – Wikipedia,
Pyridine | C5H5N – PubChem