Electric Literature of 7314-86-5,Some common heterocyclic compound, 7314-86-5, name is 1,3,5,7-Tetrabromoadamantane, molecular formula is C10H12Br4, 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 250ml three-necked flask equipped with a condenser tube5.0 g (ie 11.0 mmol) of tetrabromoadamantane and20 mL (ie, 165 mmol) of m-dibromobenzene,Condenser duct from the upper end connected to an inverted funnel 30% NaOH aqueous solution,To absorb the HBr produced by the reaction.Cold water bath at 5 ,To the reaction system was added 1.2g (ie, 4.5mmol) of AlBr3, stirring was continued under a cold water bath for 1 hour,Then remove the cold water bath,Return to room temperature for about 3 hours,The final reaction system was heated in an oil bath to 60 C for 4 hours,The reaction solution was cooled to room temperature,Pour into 100 mL of acidic ice water and stir for 1 h.After the ice is completely melted, 100 ml of methylene chloride is added to the mixture for extraction. The organic layer is washed with water until neutral, washed with saturated brine, dried over anhydrous sodium sulfate, filtered and the filtrate is concentrated. The concentrated solution is then slowly added dropwise to 100 ml Methanol, precipitation,9.31 g of a pale yellow solid was obtained in a yield of 79%.
These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 1,3,5,7-Tetrabromoadamantane, its application will become more common.
Reference:
Patent; Chinese Academy Of Sciences Physics And Chemistry Technology Institute; Chen Jinping; Li Yi; Yu Tianjun; Zeng Yi; (18 pag.)CN107266319; (2017); A;,
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