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

Active Publication Date: 2008-09-03
SHANDONG DOCRIS CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

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Method used

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Examples

Experimental program
Comparison scheme
Effect test

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.

[...

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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Abstract

The invention provides a process for preparing beta-phenylethyl bromide. The process comprises: using gasoline as a raw material, adding phenylethene, using azobisisobutyronitrile as an initiating agent for polymerization reaction, adding zinc white, strictly controlling temperature, and obtaining beta-phenylethyl bromide by the steps: reaction, distillation, cleaning, desiccation, etc. The method is simple in operation, and has a low cost, a high and steady yield and a reliable quality.

Description

technical field [0001] The invention relates to a preparation method of β-bromophenylethane, which belongs to the field of marine fine chemicals. Background technique [0002] β-Bromophenylethane, also known as 2-phenylethyl bromide, 2-bromoethylbenzene, β-bromophenylethane, β-bromoethylbenzene, is an organic synthesis intermediate widely used in Pharmaceutical, pesticide, industrial and other synthetic fields. [0003] In medicine, it can be used in the synthesis of insecticides and hypotensive agents. Industrially, it can be used as new flocculant and dispersant, excellent fiber dyeing modifier, antistatic agent for plastic, fiber and paper, viscosity regulator in photosensitive material production, ion exchange resin and exchange membrane, electroplating gloss agent, etc. Another example is widely used in the interaction of polymer self-assembled membranes, functional membranes, biomedical polymer materials (microcapsules, functional microspheres, etc.), responsive hydr...

Claims

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Application Information

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IPC IPC(8): C07C22/04C07C17/08
Inventor 杨树仁黄伟宋森鹏杨子永郝建港丁瑞林刘露露
Owner SHANDONG DOCRIS CHEM
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