Application of 5750-76-5, 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. 5750-76-5, name is 2,4,5-Trichloropyrimidine, molecular formula is C4HCl3N2, 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.
After adding a solvent N-methylpyrrolidone 12L to a 20 L double-layer glass reactor, the mechanical stirrer was turned on to stir.Then the substrate 2-(isopropylsulfonyl)aniline (199.3 g, 1 mol) was added sequentially.Potassium tert-butoxide (168.3 g, 1.5 mol),2,4,5-trichloropyrimidine (238.5 g, 1.3 mol),Zinc acetate (55.0 g, 0.3 mol),After stirring and dispersing uniformly, the temperature is raised to 120±2 C. for the heat preservation reaction;After 10 h, the reaction solution was taken for HPLC analysis (area normalization method: substrate 2-(isopropylsulfonyl)aniline was 1.18%, product 98.72%,The remaining amount is unknown impurity),The reaction was continued for 2 hours, and the reaction solution was subjected to HPLC analysis (area normalization method: substrate 2-(isopropylsulfonyl)aniline was 0.14%,99.52% of the product, the balance is unknown impurities);[0055] Stop the reaction, cool to 20-30 C and transfer to a 50L reactor;Add 8 L of isopropyl acetate under stirring, then add 30% V acetic acid aqueous solution to adjust the pH of the system to 7.5-7.8, stir 10-20pieta; – add 5.0L of purified water, stir for 8-lOmin, then let stand for 20-30 min. The liquid layer was collected, and the upper layer of isopropyl acetate was collected. The lower aqueous phase was extracted twice with isopropyl acetate, and 6.0 L of isopropyl acetate layer was added each time; all the isopropyl acetate layers were combined and washed with 10 L of saturated brine. After standing for liquid separation, the isopropyl acetate layer was collected, and then heated to 40-45 C, and 12 L of n-heptane was added dropwise with stirring, and a white solid precipitated in the system during the dropwise addition.After the addition, the temperature is lowered to 10-20 C.Then, the temperature is raised to 50-60 C, the temperature is kept 10-20pieta, and then naturally cooled to room temperature, filtered, and the filter cake is collected and dried under reduced pressure at 40-45 C to obtain 318.1 g of an off-white solid, the yield is 92.1%;The purity of 2,5-dichloro-N-[2-(isopropylsulfonyl)phenyl]pyrimidin-4-amine in white solid was 99.88%, and the unreacted substrate 2-(isopropylsulfonate) was detected by HPLC. Acyl) aniline 0.04%, the balance is unknown impurities
While traditionally a conservative industry, chemical producers will need to modernize their PR strategies to stay relevant.we look forward to future research findings about 5750-76-5, 2,4,5-Trichloropyrimidine.
Reference:
Patent; Liu Gengxi; Chen Lanhua; Ji Hui; Li Jing; Liang Li; (8 pag.)CN109020898; (2018); A;,
Pyrimidine | C4H4N2 – PubChem,
Pyrimidine – Wikipedia