Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 60811-21-4, name is 4-Bromo-2-chloro-1-fluorobenzene, A new synthetic method of this compound is introduced below., Quality Control of 4-Bromo-2-chloro-1-fluorobenzene
A dry, argon-flushed Schienk-flask equipped with a magnetic stirrer and a septum was charged with 20 mL freshly titrated iPrMgClLiCI (1.24 M in THE, 1.0 equiv.) to which 3.8 mL of diisopropylamine (1.1 equiv.) was added dropwise at 25 00. The reaction mixture was stirred at this temperature until gasevolution was completed (ca. 48 h). The formed precipitate was dissolved with additional dry THE. The fresh solution of iPr2NMgCILiCI in THE was titrated at 25 00 with benzoic acid and 4- (phenylazo)diphenylamine as an indicator. A concentration of 0.59 M was obtained.To a solution of 4-bromo-2-chloro-1 -fluoro-benzene (0.209 g, 1 .00 mmol) in THE (1 mL) was added iPr2NMgCILiCI (0.59 M, 3.39 ml, 2.00 mmol) at 25 00 and the resulting mixture was stirred for 15 mm at25 c Hexachloro-2-propanone (0.397 g, 1 .50 mmol) was added at 0 00 and the mixture was stirred for15 mm. The resulting mixture was then quenched with sat. aq. NH4CI, extracted with ethyl acetate and dried over anhydrous Na2SO4. After filtration, the solvent was removed in vacuo. Quantitative GO measurement showed that the ratio between 5-bromo-1 ,3-dichloro-2-fluoro-benzene and regioisomer is about 12:1. Purification by flash column chromatography (Si02, i-hexane) furnished 5-bromo-1 ,3-dichloro-2-fluoro-benzene (0.190 g) as a colorless oil.
The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.
Reference:
Patent; SYNGENTA PARTICIPATIONS AG; SMITS, Helmars; KNOCHEL, Paul; KLATT, Thomas; BECKER, Matthias; (18 pag.)WO2016/58895; (2016); A1;,
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