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Industrial method for preparing beta-ionone

A technology of ionone and pseudo-ionone, applied in the fields of medicine and chemical industry, can solve problems such as difficulty and achieve the effect of preventing local overheating

Inactive Publication Date: 2004-06-30
SHANGHAI INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it is difficult to achieve industrial production

Method used

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  • Industrial method for preparing beta-ionone

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Experimental program
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Effect test

Embodiment 1

[0013] Add 1100 liters of acetone, 260 liters of water, and 25 liters of 30% NaOH solution into the reaction kettle, and stir evenly. At 20° C., 170 kg of citral (content ≥ 95.0%) was added dropwise within 2 hours. After the addition was complete, the reaction was continued for 2 to 4 hours, during which samples were taken for chromatographic analysis every half hour. When the conversion rate of citral is >99.0%, neutralize with acetic acid to PH = 6.0-6.5, let stand to separate layers, separate to remove the water layer, and collect and recover acetone. The organic layer was evaporated to remove the solvent to obtain the crude pseudoionone, and the fraction at 104-109°C / 240Pa was collected by vacuum distillation to obtain 201.3 kg of the finished pseudoionone with a content of 92.2% and a yield of 90.8%.

[0014] 120 liters of 6 # Solvent oil, 5 liters of methanol, 160 liters of concentrated sulfuric acid, stir evenly, cool to -18°C, add 55 kg of the above-mentioned pseudo-i...

Embodiment 2

[0017] Add 800 liters of acetone, 260 liters of water, and 25 liters of 30% NaOH solution into the reaction kettle, and stir evenly. At 28° C., 250 kilograms of litsea cubeba oil (containing citral 67.0%) was added dropwise while stirring within 2 hours. After the addition is complete, continue to react for 2 to 4 hours, during which every half hour, samples are taken for chromatographic analysis. When the conversion rate of citral is >95.0%, neutralize with acetic acid to PH = 6.5-7, let the layers stand, and separate the water layer (collect it separately and recover acetone). The organic layer was evaporated to remove the solvent to obtain the crude product of pseudo-ionone, and the fraction at 110-117°C / 525Pa was collected by vacuum distillation to obtain 197.4 kg of the finished pseudo-ionone with a content of 90.2% and a yield of 84.2%.

[0018] 120 liters of 6 # Solvent oil, 5 liters of methanol, 160 liters of concentrated sulfuric acid, stirred and cooled to -12~-18°...

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Abstract

The industrial preparation method of high-purity beta-ionone is characterized by that 1. regulating dose of acetone, water and alkali to make the condensation reaction of citral and acetone be implemented under the condition of approaching to homogeneous phase, its reaction condition is moderate, reaction time is short and yield is high; 2. when the pseudo ionone is undergone the process of cyclization, at the same time the carbon dioxide ice is added so as to effectively prevent reaction system from local overheating and make the selectivity for forming beta-ionone be greater than 99%. Said invention can obviously raise product quality and yield, in the product the beta-ionone content is greater than or equal to 96.0%, alpha-ionone content is less than or equal to 1.0% and the yield is up to 72.0-85.0%.

Description

technical field [0001] The invention relates to an industrial preparation method of high-purity β-ionone, which belongs to the fields of chemical industry and medicine. Background technique [0002] β-ionone is a spice with wide application. High-purity β-ionone (β-body ≥ 95.0%, α-body ≤ 2.0%) is the main raw material for the production of vitamin A in the pharmaceutical industry. The synthesis of β-ionone is formed by condensation of citral and acetone to generate pseudoionone, and then cyclization of pseudoionone under acidic conditions. [0003] Due to the change in position of the ionone double bond, the product is usually a mixture of α- and β-ionones: [0004] [0005] There are many patent documents about β-ionone, most of which revolve around ① improving the yield of pseudo-ionone in the condensation reaction, and ② increasing the content of β-ionone in the cyclization product to meet the needs of the pharmaceutical industry. Regarding the condensation reaction,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/72C07C49/21
Inventor 陆庆宁顾建生田钦孙小玲周祖新
Owner SHANGHAI INST OF TECH
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