Method for preparing beta-bromine ethylbenzene
A technology of bromophenylethane and styrene, which is applied in the field of preparation of β-bromophenylethane, can solve the problems that are not conducive to industrial production, and achieve the effects of low cost, simple operation and clear mechanism
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example 1
[0027] (1) Add gasoline 300g (containing 95% pure) to a 1000ml four-neck flask with an electric stirrer, slowly heat up, and simultaneously add styrene 100g (0.96mol) and azobisisobutyronitrile to the dropping funnel 3 g (0.018 mol). When the temperature reaches 84°C, add 1.5g (0.009mol) of azobisisobutyronitrile, start to add 10g (0.096mol) of styrene dropwise under mechanical stirring, and pass hydrogen bromide gas, cool down to 80°C, and slowly add Styrene 90g (0.864mol), after 2 hours, when the temperature was naturally lowered to 79°C, the flow of hydrogen bromide gas was stopped, and a light beige transparent solution was obtained.
[0028] After testing, the content of α-bromophenylethane and styrene is less than 1%.
[0029] (2) Raise the temperature to 138°C, gasoline evaporates completely, cool down to 118°C, add 1 g (0.012 mol) of zinc oxide to a four-necked flask, raise the temperature to 142°C, react for 3 hours, stop stirring to obtain crude β-bromostyrene.
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example 2
[0034] (1) Add gasoline 300g (containing 90% pure) to a 1000ml four-necked flask with an electric stirrer, slowly heat up, and simultaneously add styrene 95g (0.91mol) and azobisisobutyronitrile to the dropping funnel 1 g (0.006 mol). When the temperature reaches 79°C, add 0.5 g (0.003 mol) of azobisisobutyronitrile into the four-neck flask, start stirring, start to add 10 g of styrene dropwise and pass hydrogen bromide gas. The temperature was raised to 82°C, and 85g (0.814mol) of styrene was slowly added dropwise. After 1.5h, the dropwise addition was completed. When the temperature was naturally lowered to 80°C, the flow of hydrogen bromide gas was stopped to obtain a light beige transparent solution.
[0035] After testing, α-bromophenylethane > 1%, styrene content > 1%
[0036] (2) Raise the temperature to 135°C, gasoline evaporates completely, cool down to 120°C, add 1.2g (0.015mol) of zinc oxide into the four-neck flask, raise the temperature to 140°C, react for 2.5h, ...
example 3
[0041] (1) Add gasoline 250g (containing 90% pure) to a 1000ml four-neck flask with an electric stirrer, slowly heat up, and add styrene 95g (0.91mol) and azobisisobutyronitrile to the dropping funnel at the same time 1 g (0.006 mol). When the temperature reaches 80°C, add 0.5 g (0.003 mol) of azobisisobutyronitrile into the four-neck flask, start stirring, start to drop 10 g of styrene and pass hydrogen bromide gas. The temperature was raised to 82°C, and 85g (0.814mol) of styrene was slowly added dropwise, and the dropwise addition was completed in 75 minutes. When the temperature was naturally lowered to 80°C, the flow of hydrogen bromide gas was stopped to obtain a yellow transparent solution.
[0042] After testing, α-bromophenylethane> 5%, styrene content> 1%.
[0043] (2) Raise the temperature to 140°C, gasoline evaporates completely, cool down to 118°C, add 2.5g (0.03mol) of zinc oxide into the four-neck flask, raise the temperature to 140°C, react for 2 hours, stop s...
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