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Preparation method of lyral

A technology of lyral and acrolein, which is applied in the field of preparation of lyral, can solve the problems of waste acid corrosion, environmental pollution, cumbersome operation steps, etc., and achieve few by-products, high yield and purity, and excellent reaction conditions mild effect

Active Publication Date: 2012-07-04
格林生物科技股份有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the Lewis acid catalysis method can reduce the reaction temperature, the reaction product needs to be post-treated, such as removing the catalyst, removing the organic solvent, etc., not only the operation steps are cumbersome, but also a large amount of waste acid will be generated to corrode the equipment and pollute the environment

Method used

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  • Preparation method of lyral
  • Preparation method of lyral
  • Preparation method of lyral

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preparation example Construction

[0026] The invention provides a kind of preparation method of lyral, comprising the following steps:

[0027] a) Myrcenol is heated to 50°C to 130°C;

[0028] b) adding acrolein dropwise to the myrcenol obtained in step a), controlling the temperature during the dropping process to be 50° C. to 130° C., and continuing the reaction after the dropwise addition to obtain neoliral.

[0029] In the present invention, firstly, the temperature of myrcenol is raised to 50°C to 130°C, that is, to the reaction temperature of myrcenol and acrolein, so that the subsequent dropwise added acrolein can immediately react with myrcenol, and the temperature is preferably 70°C ~120°C, more preferably 100°C to 110°C.

[0030] Myrcenol is a diene body with a conjugated double bond, which is prone to self-polymerization. In order to prevent myrcenyl from self-polymerization, the myrcenol preferably contains a polymerization inhibitor, and the polymerization inhibitor is preferably p-phenylene. Di...

Embodiment 1

[0045] Add 539g (3.5mol) myrcenol and 0.539g hydroquinone in the 1000mL four-necked flask that thermometer, mechanical stirring device and reflux condenser are equipped with, be heated to 110 ℃; In described myrcenol, dropwise add 235g ( 4.2 mol) of acrolein was added dropwise for 6 hours. During the dropwise addition, the reaction bottle was placed in a freezing tank, and the temperature of the reaction bottle was kept at 110°C to 130°C; after the addition of acrolein was completed, the reaction was continued for 1h to obtain the reaction mixture;

[0046] The reaction mixture is washed three times with 200g deionized water to obtain the crude product of 770g lyral, and the lyral is carried out to gas chromatography analysis, wherein the content of lyral is 96.6%; Temperature below 2mmHg carries out rectification, collects the cut between 120 ℃~125 ℃, obtains 616g lyral.

[0047] Described lyral is carried out gas chromatography analysis, the result sees figure 1 with fig...

Embodiment 2

[0051] Add 539g (3.5mol) myrcenyl alcohol and 0.539g hydroquinone in the 1000mL four-necked flask that thermometer, mechanical stirring device and reflux condenser are equipped with, be heated to 110 ℃; In described myrcenyl alcohol, dropwise add 216g ( 3.86 mol) of acrolein, added dropwise for 6 hours. During the dropwise addition, the reaction bottle was placed in a freezing tank, and the temperature of the reaction bottle was kept at 110°C to 130°C; after the dropwise addition of acrolein was completed, the reaction was continued for 1 hour to obtain mixture;

[0052] The reaction mixture is washed three times with 180g deionized water to obtain the crude product of 761g lyral, and the lyral is carried out to gas chromatography analysis, wherein the content of lyral is 95.2%; Temperature below 2mmHg, carry out rectification, collect the distillate between 120 ℃~125 ℃, obtain 605g lyral.

[0053] The lyral was analyzed by gas chromatography, and its main peaks appeared at 1...

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Abstract

The invention provides a preparation method of lyral. The method comprises the following steps of: a) heating myrcenol to 50-130 DEG C; and b) dropwise adding acrolein in the myrcenol obtained in the step a), controlling the temperature to 50-130 DEG C in the dropwise adding process, and continuously reacting after dropwise adding to obtain lyral. By controlling the addition mode and addition temperature of acrolein, myrcenol and acrolein can perform a Diels-Alder reaction without adopting high temperature and high pressure or an Lewis acid catalyst and an organic solvent, the reaction conditions are mild and by-products are fewer. As high temperature and high pressure are not required, the requirements on the reaction equipment are low and the cost of lyral can be increased; and as the Lewis acid catalyst is not required, the complicated post-treatment processes are omitted and a lot of waste acid can not be generated to corrode the equipment and pollute the environment.

Description

technical field [0001] The invention belongs to the technical field of biomass processing, and in particular relates to a preparation method of lyral. Background technique [0002] Neoliral, the English name is Lyral, the chemical name is p-(m)-(4-hydroxy-4-methylpentyl)-3-cyclohexene-1-carbaldehyde, and the molecular formula is C 12 h 22 o 2 , the molecular weight is 210.32, and the structural formula is shown in formula (I) or formula (II). Lilial is a colorless viscous liquid with a light, sweet fragrance of rabbit ear grass and a good fragrance of lily of the valley. The fragrance is stable and long-lasting. Fragrance of the product. [0003] [0004] Myrcenol is a compound prepared based on renewable resources. Its typical preparation process is as follows: turpentine oil is separated to obtain β-pinene, β-pinene is cracked to obtain myrcene, and myrcene is converted into myrcene under the protection of sulfur dioxide. Sulfone and myrcene sulfone are hydrated wi...

Claims

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Application Information

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IPC IPC(8): C07C47/46C07C45/69
Inventor 胡建良白传伟杨海宽张居宾韦国宝范宇鹏
Owner 格林生物科技股份有限公司
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