In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 25252-00-0 as follows. Recommanded Product: 25252-00-0
Tetrahydrofuran (99.7g) and sodium borohydride (15.2g, 0.4mol) were added to the reaction flask at 10-25C.A solution of 2-bromo-5-iodobenzoic acid (109.4 g, 0.34 mol, prepared in Example 2) in tetrahydrofuran (151 g) was slowly added dropwise.At 10-30C, a solution of sulfuric acid (16.4 g) in tetrahydrofuran (25 g) was added dropwise to the reaction vessel. After the addition was completed, the reaction was performed at room temperature for 2 hours. Then, it was heated to reflux 66C, refluxed for 2 hours, and then lowered to room temperature. 5% hydrochloric acid (235 g) was slowly added dropwise and THF was distilled off under reduced pressure (-0.01 MPa).Add 326.7 g of MTBE and 222.7 g of water to dissolve the solid, cool to 15-25C, separate the layers, and evaporate the organic layer under reduced pressure (-0.095 MPa).Toluene (108.8 g) and water (108.8 g) were added and the mixture was warmed to 60C for 1 h, reduced to 18-22C and filtered. After drying, 89.1 g of an off-white solid product was obtained with a measured content of >99% and a yield of 85.1%.
According to the analysis of related databases, 25252-00-0, the application of this compound in the production field has become more and more popular.
Reference:
Patent; Jinkai (Liaoning) Chemical Co., Ltd.; Wang Yongcan; Zhang Hong; Li Zhenwei; Zhao Yang; Zhang Guifang; Song Tongji; Hu Zhenzhu; Huang Fengting; (8 pag.)CN107954861; (2018); A;,
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