Adding a certain compound to certain chemical reactions, such as: 138526-69-9, name is 1-Bromo-3,4,5-trifluorobenzene, belongs to bromides-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 138526-69-9, Safety of 1-Bromo-3,4,5-trifluorobenzene
To a reaction vessel under a nitrogen atmosphere, 1-bromo-3,4,5-trifluorobenzene (10.7 g) and diethyl ether (150 ml) were added, and cooling was carried out to -50C. Thereto, a n-butyllithium (1.57 M) n-hexane solution (30.7 ml) was added dropwise in a temperature range of -50C to -45C, and stirring was carried out for another 1 hour. Then, after cooling to -74C, a diethyl ether (20.0 ml) solution of compound (T-3) (7.47 g) was added dropwise in a temperature range of -74C to -70C, and stirring was carried out for 4 hours while returning to room temperature. The resultant reaction mixture was poured into ice water (200 ml), and mixing was carried out. Toluene (200 ml) was added to separate layers into an organic layer and an aqueous layer, and an extraction operation was performed. The resultant organic layer was sequentially washed with a 1 N hydrochloric acid solution, a saturated aqueous solution of sodium hydrogencarbonate and water, and drying over anhydrous magnesium sulfate was carried out. The resultant solution was concentrated under reduced pressure, and a residue was purified by fractionation by means of column chromatography (silica gel; heptane), and further purified by recrystallization from a heptane/Solmix A-11 mixed solvent, and thus (E)-4-[1,2-difluoro-2-(3,4,5-trifluorophenyl)vinyl]-3-fluoro-4′-pr opylbiphenyl (1-1-1) (3.75 g) was obtained. The yield based on compound (T-3) was 36%. Chemical shifts according to 1H-NMR analysis were as described below, and the compound obtained could be identified to be (E)-4-[1,2-difluoro-2-(3,4,5-trifluorophenyl)vinyl]-3-fluoro-4′-pr opylbiphenyl. Chemical shifts delta (ppm; CDCl3); 7.58 (dd, J = 7.80 Hz, J = 7.65 Hz, 1H), 7.53 (d, J = 8.15 Hz, 2H), 7.50 – 7.37 (m, 4H), 7.29 (d, J = 8.10 Hz, 2H), 2.65 (t, J = 7.85 Hz, 2H), 1.75 – 1.64 (m, 2H), 0.98 (t, 7.45 Hz, 3H). A phase transition temperature of compound (1-1-1) obtained was as described below. Phase transition temperature: C 66.2 SA 95.2 N 116 I.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-3,4,5-trifluorobenzene, and friends who are interested can also refer to it.
Reference:
Patent; JNC Corporation; JNC Petrochemical Corporation; EP2522649; (2012); A1;,
Bromide – Wikipedia,
bromide – Wiktionary