Category: 6320-40-7

Synthetic Route of 6320-40-7, These common heterocyclic compound, 6320-40-7, name is 1,3,5-Tribromo-2-methylbenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Synthesizing of Intermediates A and B 3.3g (10 mmol) of 2,4,6-tribromotoluene was dissolved in 30 mL of diethylether. The resulting solution was cooled to -78 C and 4.4mL (11 mmol) of normalbutylithium (2.5M in Hexane) was slowly added thereto. The resulting solution was stirred at -78C for one hour and 1.48g (11 mmol) of cooper chloride (II) was added thereto at -78C. The reactant product was stirred for 5 hours and cleaned using distilled water and ethylacetate at room temperature. The cleaned ethylacetate layer was dried over MgSO4 and dried under a reduced pressure, thereby producing a crude-product. The pre-product was refined through a column chromatography and the refined result was recrylstallized in dichloromethane and hexane, thereby producing white solid intermediates A and B. Amounts of A and B were 622 mg (yield 25%) and 746 mg (yield: 30%), respectively. Intermediate A : 1H NMR (CDCl3, 400MHz) delta (ppm) 7.74 (d, 4H), 7.18 (d, 4H), 2.06 (s, 6H); 13C NMR (CDCl3, 100MHz) delta (ppm) 142.8, 134.9, 134.5, 131.1, 126.4, 119.4, 19.9 Intermediate B : 1H NMR (CDCl3, 400MHz) delta (ppm) 7.60 (s, 4H), 2.61 (s, 6H); 13C NMR (CDCl3, 100MHz) delta (ppm) 138.3, 137.2, 129,9, 125.8, 23.5

The synthetic route of 6320-40-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung SDI Co., Ltd.; EP1752442; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 6320-40-7, These common heterocyclic compound, 6320-40-7, name is 1,3,5-Tribromo-2-methylbenzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Synthesizing of Intermediates A and B 3.3g (10 mmol) of 2,4,6-tribromotoluene was dissolved in 30 mL of diethylether. The resulting solution was cooled to -78 C and 4.4mL (11 mmol) of normalbutylithium (2.5M in Hexane) was slowly added thereto. The resulting solution was stirred at -78C for one hour and 1.48g (11 mmol) of cooper chloride (II) was added thereto at -78C. The reactant product was stirred for 5 hours and cleaned using distilled water and ethylacetate at room temperature. The cleaned ethylacetate layer was dried over MgSO4 and dried under a reduced pressure, thereby producing a crude-product. The pre-product was refined through a column chromatography and the refined result was recrylstallized in dichloromethane and hexane, thereby producing white solid intermediates A and B. Amounts of A and B were 622 mg (yield 25%) and 746 mg (yield: 30%), respectively. Intermediate A : 1H NMR (CDCl3, 400MHz) delta (ppm) 7.74 (d, 4H), 7.18 (d, 4H), 2.06 (s, 6H); 13C NMR (CDCl3, 100MHz) delta (ppm) 142.8, 134.9, 134.5, 131.1, 126.4, 119.4, 19.9 Intermediate B : 1H NMR (CDCl3, 400MHz) delta (ppm) 7.60 (s, 4H), 2.61 (s, 6H); 13C NMR (CDCl3, 100MHz) delta (ppm) 138.3, 137.2, 129,9, 125.8, 23.5

The synthetic route of 6320-40-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Samsung SDI Co., Ltd.; EP1752442; (2007); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

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 6320-40-7 as follows. Application In Synthesis of 1,3,5-Tribromo-2-methylbenzene

Synthesis of Intermediates H and I; 2,4,6-tribromotoluene (3.3 g, 10 mmol) was dissolved in diethylether (30 ml). The reaction solution was cooled to -78 C., and n-butyllithium (4.4 ml, 11 mmol, 2.5M in hexane) was gradually added thereto. The reaction mixture was stirred at -78 C. for one hour, and copper chloride (II) (1.48 g, 11 mmol) was added thereto at -78 C. The reaction solution was stirred for five hours, and washed with distilled water and ethylacetate at room temperature. The obtained ethylacetate layer was dried over MgSO4 and then dried under a reduced pressure to obtain a crude product. The crude product was purified by silica gel column chromatography and recrystallized from dichloromethane and hexane to give intermediate H (622 mg, yield: 25%) and an intermediate I (746 mg, yield: 30%) as white solids. The structures of intermediates H and I were determined by 1H NMR. Intermediate H: 1H NMR (CDCl3, 300 MHz) delta (ppm) 7.74 (d, 4H), 7.18 (d, 4H), 2.06 (s, 6H); 13C NMR (CDCl3, 100 MHz) delta (ppm) 142.8, 134.9, 134.5, 131.1, 126.4, 119.4, 19.9. Intermediate I: 1H NMR (CDCl3, 300 MHz) delta (ppm) 7.60 (s, 4H), 2.61 (s, 6H); 13C NMR (CDCl3, 100 MHz) delta (ppm) 138.3, 137.2, 129, 9, 125.8, 23.5.

According to the analysis of related databases, 6320-40-7, the application of this compound in the production field has become more and more popular.

Reference:
Patent; Samsung SDI Co., Ltd.; US2008/174237; (2008); A1;,
Bromide – Wikipedia,
bromide – Wiktionary

Electric Literature of 6320-40-7, A common heterocyclic compound, 6320-40-7, name is 1,3,5-Tribromo-2-methylbenzene, molecular formula is C7H5Br3, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

In a 100 mL agate ball mill jar, 3.29 g (10 mmol)2,4,6-tribromotoluene, 0.0010 g (0.0010 mmol) 5,10,15,20-tetrakis(2,3,4,5,6-pentafluorophenyl)porphyrin cobalt (II), 6.44 g (50 mmol) 70% t-butyl hydroperoxide aqueous solution and 16.45 g of anhydrous sodium sulfate were mixed uniformly, and the ball mill tank was sealed. At room temperature, the ball milling reaction was performed at a speed of 800 rpm for 16.0 h, and the ball milling was stopped every 1.0 h to release the gas in the ball milling tank. After completion of the reaction, the obtained reaction mixture was dissolved in 30 mL of absolute ethanol and stirred at room temperature for 30.0 min. Filter, wash the obtained filter cake with 2 × 10 mL of absolute ethanol, combine the ethanol solutions, and make the resulting ethanol solution to 100 mL. 20 mL of the obtained solution was removed, desolvated under reduced pressure, and the obtained reaction mixture was separated by column chromatography (V cyclohexane: V ethyl acetate = 4: 1 to 1: 4). The conversion of 2,4,6-tribromotoluene was 31%, and the selectivity of 2,4,6-tribromobenzoic acid was 99%. No other significant oxidation products were detected.

The synthetic route of 6320-40-7 has been constantly updated, and we look forward to future research findings.

Reference:
Patent; Zhejiang University of Technology; Shen Haimin; Qi Bei; She Yuanbin; (18 pag.)CN110563590; (2019); A;,
Bromide – Wikipedia,
bromide – Wiktionary