With the rapid development and complex challenges of chemical substances, new drug synthesis pathways are usually the most effective.108-55-4,Dihydro-2H-pyran-2,6(3H)-dione,as a common compound, the synthetic route is as follows.
Treatment of aluminum trichloride:Anhydrous aluminum trichloride (purchased from Sinopharm Group Chemical Reagent Co., Ltd.,Product number 10000862). The aluminum trichloride was pulverized in a mortar,The aluminum trichloride fine particles were obtained by sieving with a 40 mesh sieve,The fine particles were then placed at 110 C C bake lh to a large number of white smoke smoke,And the mixture was cooled to room temperature under a nitrogen atmosphere.Preparation of 4- (4-fluorobenzoyl) butanoic acid:Under the protection of nitrogen, the treated aluminum chloride was added to the 500 mL three-necked flask according to the raw material ratio of Table 1,Fluorobenzene and organic solvent 100mL, stirring and evenly, the three-necked flask placed in the ice bath, to which dropping glutaric anhydride solution, which, glutaric anhydride solution used in the same solvent and dissolved fluoride, the amount of 48mL, Lh. After dropping, the ice bath was withdrawn, the room temperature was recovered, and the reaction was carried out according to the reaction conditions in Table 2. After completion of the reaction,The reaction was poured into a 2 L beaker and ice was added. The pH was adjusted to 1 by the addition of dilute hydrochloric acid (2N)Filtration gave the crude product, in which the brown red viscous material was aluminum complex;The crude product was redissolved twice in 600 mL of saturated aqueous NaHC03 solution ( & 110) 3 in an appropriate excess)Heated in boiling water bath for 2 hours to have a large number of red sticky material floating on the surface,While filtering the pale yellow solution,And adding concentrated hydrochloric acid to adjust pH to 1,A large number of bubbles emerge,A white solid precipitation,Filtering, washing with cold water, drying,To give 4- (4-fluorobenzoyl) butanoic acid., 108-55-4
The synthetic route of 108-55-4 has been constantly updated, and we look forward to future research findings.
Reference£º
Patent; ZHEJIANG NHU CO LTD; Zhejiang University; ZHANG, YUHONG; JU, LONG; YU, MING; DUAN, XIAOTING; (8 pag.)CN103694111; (2016); B;,
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