According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.
Reference of 2972-52-3, 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. 2972-52-3, name is 2,4-Dichloro-5-pyrimidinecarbonyl chloride, molecular formula is C5HCl3N2O, 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 3 Synthesis of 5-carboxyamide-2,4-dichloropyrimidine To a 2 L round bottom flask equipped with water condenser and a CaCl2 drying tube, 2,4-dihydroxypyrimidine (25 g, 0.16 mole) was added to PCl5 (117 g, 0.56 mole), and POCl3 (250 ml, 2.6 mole). The mixture was heated at 115 C. overnight to give a clear, slightly light yellow solution. The mixture was cooled to room temperature, and was concentrated under reduced pressure to give pale yellowish oil. To this oil, anhydrous 1,4-dioxane (300 ml) was added and the mixture was cooled to 0 C. in an ice/water bath. 35 ml of NH3 in water (28%) was added dropwise to the mixture with stirring, temperature was kept below 5 C. The mixture changed from clear to white with precipitate forming, and was stirred for 1 hour at 0 C., reaction was followed by TLC (1:1 Hexanes:Ethyl Acetate). Ethyl acetate (700 ml) and water (500 ml) were added to the mixture, the 2 layers were separated. The organic layer was dried with Na2SO4, and filtered. The solution was concentrated under reduced pressure to give a light yellow solid. This light yellow solid was sonicated with methylene chloride (200 ml), and filtered to give a pale yellow solid (16 g). This pale yellow solid was dissolved into ethyl acetate (1.5 L) and washed with sat. NaHCO3 (500 ml). The organic layer was dried with Na2SO4, filtered, and concentrated under reduced pressure to give 13.1 g of product as a white solid (44% yield). 1H NMR (DMSO-d6, 300 MHz): delta 8.86 (s, 1H), 8.14 (bs, 1H), 8.02 (bs, 1H).
According to the analysis of related databases, 2972-52-3, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Holland, Sacha; Kolluri, Rao; Alvarez, Salvador; Duncton, Matthew; Singh, Rajinder; Zhang, Jing; Masuda, Esteban; US2012/22092; (2012); A1;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia