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Synthesis method of thio-menthone perfume

A technology of thiomenthone and a synthesis method, applied in the field of fragrances, can solve the problems of large equipment investment, increased equipment manufacturing cost and operational difficulty, severe corrosion of steel equipment and the like

Inactive Publication Date: 2010-06-16
HUABAO FLAVOURS & FRAGRANCES CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this method is difficult to implement in industry, and there are many problems, such as: 1, it must need large, medium-sized steel pressure vessel equipment, and the equipment investment is large; 2, the H in the process 2 S is very corrosive to steel equipment, and the maintenance and depreciation costs of equipment are high; 3. The process requires the reaction temperature to reach -80°C, which requires a lot of energy consumption; 4. The internal temperature of large and medium-sized pressure vessels must reach -80°C , it is also difficult in design, which will increase the manufacturing cost and operation difficulty of the equipment
The literature (Flavour & Fragrance J., 1993, Vol.8 (5), 289-294) has reported that, for example, use aluminum trichloride Lowis acid to induce, which is conducive to H 2 Electrophilic addition of S, but only 9% yield of thiomenthone

Method used

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  • Synthesis method of thio-menthone perfume
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  • Synthesis method of thio-menthone perfume

Examples

Experimental program
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Embodiment 1

[0093] In the flask equipped with lye tail gas absorbing device, add the pulverulent crude oil of the isopulegone (23g) of 25ml content 80% by weight. Then feed HCl gas at a flow rate of 70ml / min until saturation, and the reaction solution will increase in weight by about 6g, and proceed to the next reaction immediately. Add 120ml of dehydrated ethanol in the 500ml three-neck flask equipped with a stirrer, a thermometer, a reflux condenser, and a dropping funnel inside, then add 3.5g of sodium metal cut into small pieces, and treat that the sodium metal is completely dissolved in reflux. Cool to room temperature, pass through H 2 S gas until PH=7.5. Cool the sodium mercaptolate solution to 10°C, then add the freshly prepared chloromenthone solution dropwise therein for about one hour, and then stir at room temperature for 2 hours. After the reaction, 100ml of water and 100ml of ether were added for washing and extraction, the phases were separated, and the separated ether ph...

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Abstract

The invention relates to a synthesis method of thio-menthone perfume, which comprises the steps of: preparation of chloro-menthone, preparation of sodium hydrosulfide, preparation of crude thio-menthone, rectification of the crude thio-menthone and the like. Compared with the prior art, the method is convenient for industrial implementation, less in equipment investment and easy in operation; the technique has highest yield in the preparation of the thio-menthone under the technical condition of normal pressure and normal temperature; meanwhile, the method solves the problems of high equipment investment, strong equipment corrosion, high power consumption, hard operation and the like caused by the technology for preparing the thio-menthone at high pressure and low temperature.

Description

【Technical field】 [0001] The invention belongs to the technical field of spices, and more specifically, the invention relates to a method for synthesizing thiomenthone spices. 【Background technique】 [0002] The chemical name of thiomenthone (1) is 2-(1-mercapto-1-methylethyl)-5-methylcyclohexanone (2-(1-mercapto-1-methylethyl)-5-methyl- cyclohexanone), as represented by the following formula (1). It is one of the important fragrance raw materials in the fragrance industry. Its smell in its pure state is not pleasant, but once diluted, it has a strong fruity, green, toasty aroma, slightly warm and sweet, even minty, It plays an important role in the preparation of blackcurrant, peach, vegetable and other food flavors. Thiomenthone is also widely used in the preparation of toothpaste flavor and characteristic aroma of daily chemical products. The trace application of thiomenthone in tobacco flavors can enhance the flavors of green, sweet and fruity. The FEMA number for T...

Claims

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Application Information

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IPC IPC(8): C07C323/22C07C319/02
Inventor 施友钟罗昌荣
Owner HUABAO FLAVOURS & FRAGRANCES CO LTD
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