621-38-5, 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 621-38-5 as follows.
Example 43-chloro -2 the same-acetamido […] synthesis ofTo 10 ml reaction flask by adding 3-bromo(acetylaniline) (0.2mmol, 42 . 81 mg), palladium acetate (0.002mmol, 0 . 45 mg), 3- chloroiodobenzene (0.22mmol, 52 . 46 mg), K3PO4(0.6mmol, 127 . 36 mg), silver acetate (0.3mmol, 50 . 07 mg), TFA (0.1mmol) and DCE (2 ml), for 90 C reaction under the conditions, the TLC reaction monitoring, when the temperature is reduced to the room temperature, adding phenylo boric acid (1.2mmol, 29 . 26 mg) with the ligand two phenol (0.004mmol, 1 . 07 mg), 80 C to continue reaction, the end point of the detection reaction TLC. When the reaction to room temperature, add 5 ml ethyl ether, the reaction solution is poured into the separatory funnel, using 5 ml ethyl ether washing reaction bottle, and then merged into the separatory funnel in ethyl ether, is added to the separatory funnel in 10 ml saturated NaCl solution, oscillating, liquid, so then to 10 ml ¡Á 2 of ethyl ether extraction, combined with the phase, adding anhydrous sodium sulfate for drying, filtering, vacuum screwed out of the solvent, with petroleum ether and ethyl acetate 3:1(v/v) as the mobile phase, rapid column separation, get the pure product white solid 3-chloro -2 the three-acetamido […] biphenyl, yield 86.5%.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 621-38-5, and friends who are interested can also refer to it.
Reference:
Patent; Heilongjiang University; Chu, Wenyi; Ren, Limin; Sun, Zhizhong; Guan, Dinghui; Han, Lu; Wang, Lulu; Shi, Yang; (10 pag.)CN104003895; (2016); B;,
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