Synthesis method of high-content dihydroisojasmone spice

A technique for dihydrojasmone and a synthetic method, which is applied in the field of synthesis of high-content dihydrojasmone spices, can solve the problems of harsh reaction conditions, complicated operation, and low total yield, and achieve high total yield and simple steps. Effect

Inactive Publication Date: 2020-06-19
ANHUI HYEA AROMAS
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Problems solved by technology

[0003] In the prior art, the synthetic method of dihydrojasmone has multiple, mainly contains: (1) jasmone is catalytically reduced, but, the raw material source of this synthetic method and cost exist problem; (2) by acrylate and octyl Alcohol is condensed under peroxide catalysis, then dehydration rearrangement can make dihydrojasmone under phosphoric acid existence condition, but this method will produce a large amount of phosphoric acid waste water; (3) undecanedione method: combine 2,5 -Undecanedione, ethanol, and 2% sodium hydroxide solution were heated and refluxed for 6 hours under the protection of nitrogen, and the reaction solution was concentrated and then extracted with petroleum ether. Th

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  • Synthesis method of high-content dihydroisojasmone spice

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Embodiment 1

[0031] A kind of synthetic method of dihydrojasmone perfume, comprises following concrete steps:

[0032] (1) Turn on the cooling water of the integrated cooling and heating switch, control the temperature at 15-25°C, turn on the agitator, then add 280g of 2-octanol to the 500ml flask, then add 60g of acrylic acid, 15g of water and di-tert-butyl respectively Base peroxide 14g, stir well, obtain batching mixture for subsequent use;

[0033] (2) Add 2-octanol 380g in the 1500ml there-necked flask with reflux device, open the magnetic stirrer, then add catalyst boric acid 1.5g, stir;

[0034] (3) Turn on the cooling water of the reflux device, turn on the integrated cooling and heating switch, heat and control the reaction temperature at 156-160°C, then slowly add the ingredient mixture obtained in step (1) dropwise to the three-necked flask through a peristaltic pump, dropwise Keep reflux during the process, and the dropping time is controlled at 4h;

[0035] (4) After the dro...

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Abstract

The invention belongs to the technical field of spice synthesis, in particular to a synthesis method of a high-content dihydroisojasmone spice. The synthesis method comprises the following steps: by taking 2-octanol as a solvent, di-tert-butyl peroxide as an initiator and boron acid as catalyst, enabling acrylic acid and 2-octanol to be subjected to a free radical addition reaction and a reflux reaction to separate out tert-butyl alcohol and water, performing reduced pressure distillation to realize recycling of 2-octanol, collecting 5-methyl-5-hexyl-2 (3H) furanone, and rearranging and dehydrating 5-methyl-5-hexyl-2 (3H) furanone molecules under the action of a solid acid catalyst by taking white oil as a solvent to synthesize a dihydroisojasmone spice product. The synthesis method provided by the invention has the advantages of relatively simple steps, no generation of acidic wastewater and relatively high total yield. In addition, through calculation, the content of dihydroisojasmone in the product synthesized by the synthesis method provided by the invention is up to 98% or above.

Description

technical field [0001] The invention belongs to the technical field of perfume synthesis, and in particular relates to a method for synthesizing high-content dihydrojasmone perfume. Background technique [0002] The chemical name of dihydrojasmone is 2-pentyl-3-methyl-2-cyclopenten-1-one, the CAS number is 1128-08-1, also known as tetrahydropyrethrin, which has strong and fresh The aroma of jasmine and fruity fragrance, when thick, it is green with bitterness, and after dilution, it has the fragrance of jasmine. The appearance of dihydrojasmone is colorless to slightly yellow liquid, with a boiling point of 120°C / 12mmHg, a flash point of 130°C, a relative density of 0.915-0.920 (25 / 25°C), and a refractive index of 1.475-1.481 (20°C). ~10 volumes of 70% ethanol or the same volume of 80% ethanol, dissolved in oily spices. Due to the strong and long-lasting jasmine aroma and strong and mild fruity aroma of dihydrojasmone, it is often used as a fragrance raw material for cosme...

Claims

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Application Information

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IPC IPC(8): C07C45/59C07C49/647
CPCC07C45/59C07C2601/16C07D307/58C07C49/647
Inventor 王天义汪洋张政徐基龙何云飞吴旭
Owner ANHUI HYEA AROMAS
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