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;,
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