108-37-2, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 108-37-2 name is 1-Bromo-3-chlorobenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.
0.72 g (29.6 mmol) of magnesium dust was immersed in 15 mL of anhydrous tetrahydrofuran, and one iodine was added thereto, and two drops of m-chlorobromobenzene were added dropwise at room temperature. The turbidity was changed by the air gun micro-heating system, and the system was slightly boiled and dropped into 15 mL of tetrahydrofuran and 5.61 g.A mixture of (29.3 mmol) m-bromochlorobenzene was heated and refluxed for 3 hours after the dropwise addition. Decrease to room temperature and use until the next step. To a solution of the format reagent in tetrahydrofuran, 0.34 g (1.8 mmol) of cuprous iodide was added, and the mixture was stirred at room temperature for 1 hour. Slowly drip propargyl alcohol0.66 g (11.7 mmol), after completion of the dropwise addition, was heated to reflux for 24 hours. After cooling, a saturated ammonium chloride solution was added dropwise to adjust pH = 5. Extracted 3 times with 30 mL of ethyl acetate, combined organic phase, washed with saturated sodium hydrogen carbonate solution, washed with saturated sodium chloride solution, anhydrousDry over sodium sulfate. After spin-drying, 10 mL of methanol was added to the system to precipitate a solid, and the solid was taken out and distilled under reduced pressure to give 1.84 g of a pale yellow oily liquid. The yield was 92.3%.
At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-3-chlorobenzene, and friends who are interested can also refer to it.
Reference:
Patent; Hebei University of Science and Technology; Zhang Guogang; Du Wei; Zhao Yanli; Feng Xue; Song Miaomiao; Song Wei; Yang Ying; (11 pag.)CN108484535; (2018); A;,
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