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Preparation method of borneol diene

A technology for bornadiene and pinene, which is applied in the field of preparing bornadiene, can solve the problems of chlorine reaction metering difficulty, many steps and devices, unstable reaction and the like, and achieves the advantages of industrialized operation, mature technology and reduced production cost. Effect

Inactive Publication Date: 2010-10-27
NANJING FORESTRY UNIV
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Problems solved by technology

However, this study has the following disadvantages: the gas-liquid two-phase is heterogeneous, the reaction is unstable, the measurement of chlorine gas reaction is difficult, and there are many steps and devices required for simultaneous reaction.

Method used

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  • Preparation method of borneol diene
  • Preparation method of borneol diene
  • Preparation method of borneol diene

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Embodiment 1～9

[0024] In step (1), add 10ml α-pinene and 40ml solvent A in a 250mL four-neck flask equipped with a mechanical stirring device, a thermometer, and a reflux condenser, and pre-mix the liquid bromine of 10ml solvent A with a feed ratio C to form a bromine solution , immerse the reaction flask in a low-temperature bath, control the temperature E, and slowly add bromine solution dropwise to the reaction flask through a constant pressure dropping funnel while stirring at a speed of 0.25 drops / min. After the bromine solution has been added dropwise, continue After stirring for a reaction time G, the reaction was terminated; the reaction bottle was taken out to return to room temperature, and NaHCO was added 3 Wash with aqueous solution for at least 2 times, generally 3 to 4 times. At this time, the organic layer solution is light yellow to white and transparent, and then separate the liquids. Take an appropriate amount of anhydrous magnesium sulfate to remove water from the organic l...

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Abstract

The invention discloses a method for preparing borneol diene. The method comprises the following steps of: taking alpha-pinene and liquid bromine as reaction raw materials, controlling the temperature at -70 to 10 DEG C, dripping a bromine solution at constant speed when stirring, reacting for 8 to 28h and preparing crude 2,6-dibromo alkyl camphene; and taking the crude 2,6-dibromo alkyl camphene as a raw material, adding a proper solvent and a proper elimination reagent, controlling the temperature at 60 to 120 DEG C, stirring, reacting for 1 to 6h, cooling to room temperature and carrying out water washing, petroleum ether extraction and liquid division operation on reaction liquid sequentially so as to prepare the borneol diene after circulating for many times. The preparation method of the borneol diene adopts a liquid-liquid homogeneous reaction system, reduces the processes and the devices of gas generation, introduction, tail gas absorption and the like, lowers the production cost, reduces the pollution and is more beneficial to industrialized operation; and the yield of the 2,6-dibromo alkyl camphene is enhanced to 28.3 percent, the highest conversion rate of converting the 2,6-dibromo alkyl camphene to the borneol diene is 99.1 percent, and the invention has obvious economic benefit.

Description

technical field [0001] The invention relates to a compound synthesis method, in particular to a method for preparing bornadiene. Background technique [0002] Borneodiene (2,5-Bomadiene, 1,7,7-trimethylbicyclo[2,2,1]-2,5-heptadiene) is a colorless or light yellow crystal, easily soluble in toluene, soluble in In methanol, insoluble in water. Bornadiene is a chemically active bicyclic monoterpene compound, which has a similar molecular structure to norbornadiene (2,5-Norbomadiene, bicyclo[2,2,1]-2,5-heptadiene) , as attached Figure 7 Shown is the molecular structure of norbornadiene, attached Figure 6 Molecular structure of bornadiene. [0003] Norbornadiene compounds are a class of high-performance, large-capacity energy storage materials that attract attention, and have aroused great interest from researchers; biological inhibitors of norbornadiene and ethylene synthesis can be formulated as preservatives; norbornadiene Diene can also be used as a variety of olefin po...

Claims

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Application Information

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IPC IPC(8): C07C13/42C07C1/30
Inventor 曾韬窦立英李开婧杨晓琴吴振华
Owner NANJING FORESTRY UNIV
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