Reference of 327-52-6, 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 327-52-6 as follows.
N2 Protected, single-neck flask in 20ml inputs 0.4g Dppp (0.001mol, 0.1eq), 0.11g (0.0005mol, 0.05eq) of palladium acetate, acetonitrile 3g, purged three times with stirring, heated in a water bath warmed to 58 ~ 62 , for 2.5 to 3.5 hours. document.write(“”); Incubation was completed, was cooled to 30 ~ 35 , a catalyst. document.write(“”); N 2Protected, into two flasks in 50ml of 1.4g (0.01mol, 1.0eq) and itaconic acid monomethyl ester, acetonitrile 10g, stirring and mixing uniformly; was added DBU: 3.8g (0.025mol, 2.5eq), a clear solution; 2,4,5-trifluoro-bromobenzene was added: 2.32g (0.011mol, 1.1eq), stirring; N2 of replacement three times, the catalyst prepared above was added, N 2Substituted three times, under N2 protection, reaction at 80 24 hours. TLC Bi insulation test point to the raw material disappears, the reaction was complete. The reaction solution (10 mL x 3) and washed with 13% brine, dried over sodium sulfate, filtered and concentrated to a crude product of Formula 3 compounds done, purified through the column to obtain 2.3g, Yield: 83.9%. document.write(“”); Preparation of Compound 4: Example 2
According to the analysis of related databases, 327-52-6, the application of this compound in the production field has become more and more popular.
Reference:
Patent; ZHEJIANG JIUZHOU PHARMACEUTICAL CO., LTD; ZHU, GUOLIANG; HE, QIAN; QIAN, LINGFENG; XU, YINGZHOU; YAN, PUZHA; (11 pag.)CN106146340; (2016); A;,
Bromide – Wikipedia,
bromide – Wiktionary