Synthetic Route of 131860-97-4, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 131860-97-4, name is (E)-Methyl 2-(2-((6-chloropyrimidin-4-yl)oxy)phenyl)-3-methoxyacrylate, molecular formula is C15H13ClN2O4, The compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
Example 1: In a 500 mL flask equipped with a magnetic stirrer, (E)-methyl 2-(2- ((6-chloropyrimidin-4-yl)oxy)phenyl)-3-methoxyacrylate (100 g, 97 % pure, 302 mmol), 2-hydroxybenzonitrile (41 g, 341 mmol) and potassium carbonate (25.08 g, 181 mmol) were added. Water (50 mL) and /V-methyl- piperidine (2.86 g, 28.8 mmol) were added at ambient temperature, then the mixture was placed on an oil bath at ambient temperature and heating begun. The mixture was heated to 120 C over 20 min and stirring begins once the external temperature is approx. 80 C. Some gas evolution was noted. The mixture was stirred at 100 C for 5 h, under a mild reflux. The mixture was then cooled to 80 C and diluted with ethyl acetate (200 mL) and then with water (100 mL). The two phases were stirred and separated. The upper organic portion was evaporated to dryness under vacuum at 40 C. The crude residue was dissolved in methanol (200 mL) at reflux, then water (30 mL) was added slowly at that temperature. The solution was allowed to cool freely with agitation to ambient temperature over lh and the solution was seeded with 0.4 g pure azoxystrobin at 40 C. The resulting slurry was further cooled to 0 C over 20 min, and held there for a further 20 min, then the solids were recovered by suction filtration and washed with 50 mL cold methanokwater 4: 1. The filter cake was dried under vacuum at ambient temperature overnight, affording the product azoxystrobin (114.68 g, 97% pure, 91.2 % yield) as a free flowing pale brown powder.
According to the analysis of related databases, 131860-97-4, the application of this compound in the production field has become more and more popular.
Reference:
Patent; CHEMINOVA A/S; LINDSAY, Karl Bernhard; WO2014/190997; (2014); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia