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. 327-51-5, name is 1,4-Dibromo-2,5-difluorobenzene, A new synthetic method of this compound is introduced below., Computed Properties of C6H2Br2F2
Under a nitrogen atmosphere, in an 100 ml Schlenk reaction vessel, THF solution 4.5 ml (3.6 mmol) of isopropylmagnesiumbromide (manufactured by Tokyo Chemical Industry Co., Ltd., 0.80M) and THF10ml were added. The mixture was cooled to -75 C,and 2,3-dibromo-thiophene (manufactured by WakoPure Chemical Industries) 873mg (3.61mmol) was added dropwise. after aging at -75 for 30 minutes, diethyl ether solution 3.6ml (3.6mmol) of zinc chloride (Sigma Aldrich, 1.0M) was dropped. After gradually warmed to roomtemperature, the resulting white slurrymixture was concentrated under reduced pressure, to distill off the low-boilingfraction of 10ml. To the resulting white slurry liquid (3 bromothienyl-2-zinc chloride),1,4-dibromo-2,5-difluorobenzene(manufactured by Wako Pure Chemical Industries, Ltd.) 272mg (1.00mmol), tetrakis (tri phenyl phosphine) palladium as catalyst (manufacturedby Tokyo Kasei Kogyo) 39.1mg (0.0338mmol, 3.38 mol% with respect to 1,4 dibromo-2,5-difluorobenzene)and THF10ml were added. After performing reactionfor 8 hours at 60 C, the reaction vessel was water-cooled and by the addition of 3N hydrochloricacid 3ml, reaction was stopped. It was extracted with toluene and the organicphase was washed with brine, and dried with anhydrous sodium sulfate.concentrated under reduced pressure, And the resulting residue was purified bysilica gel column chromatography (from hexane,hexane / dichloromethane = 10/1),further purified by recrystallization from hexane / toluene = 6/4, to give a pale yellow solid 227mg of 1,4-di (3- bromothienyl) -2,5-difluorobenzene(52% yield).
The synthetic route of 327-51-5 has been constantly updated, and we look forward to future research findings.
Reference:
Patent; TOSOH CORPORATION; WATANABE, MAKOTO; (14 pag.)JP5790069; (2015); B2;,
Bromide – Wikipedia,
bromide – Wiktionary