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A kind of preparation method of preparing 3-methylthiopropanol from 3-methylthiopropionaldehyde

A technology of methylthiopropanol and methylthiopropionaldehyde, which is applied in the preparation of sulfides and organic chemistry, can solve the problems of reducing the reduction activity of sodium borohydride or lithium aluminum hydride, and achieve high yield, cost reduction, Effects in simple steps

Active Publication Date: 2018-08-17
BLUESTAR ADISSEO NANJING CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, commonly used solvents such as methanol, which release H during the reaction + Severely reduces the reducing activity of sodium borohydride or lithium aluminum hydride, making further reactions impossible

Method used

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  • A kind of preparation method of preparing 3-methylthiopropanol from 3-methylthiopropionaldehyde
  • A kind of preparation method of preparing 3-methylthiopropanol from 3-methylthiopropionaldehyde

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[0029] The preparation method provided by the present invention directly prepares 3-methylthiopropanol from 3-methylthiopropanal (MMP) by using a reducing agent and 3-methylthiopropanol, and the preparation method is straightforward and easy to realize industrialized quantities Produce. 3-Methylthiopropanol is a weaker acid than methanol, therefore, the reducing agent is stable in 3-Methylthiopropanol for several hours. In order to avoid thermal decomposition reaction of 3-methylthiopropanal (MMP) due to runaway heat release, special attention should be paid to the addition of reducing agent and temperature control.

[0030] In a preferred embodiment, the specific steps of the preparation method provided by the present invention are as follows: Add the reducing agent to 3-methylthiopropanol at a temperature of 0° C. to obtain a suspension. Slowly add 3-methylthiopropanal (MMP) dropwise to the obtained suspension while controlling the temperature below 20° C. to avoid side rea...

Embodiment 1

[0032] Table 1 is the influence of different solvents on the preparation of 3-methylthiopropanol from 3-methylthiopropanal (MMP). At a temperature of 0°C, an excess of 10% of the reducing agent sodium borohydride (NaBH 4 ) was added into 30mL solvent to obtain a suspension. Then, 10 g of 3-methylthiopropanal (MMP) was slowly added dropwise to the resulting suspension while controlling the temperature below 20°C. After the dropwise addition is completed, stir at room temperature, and after 3-12 hours, add HCl solution to the reaction solution for hydrolysis. After hydrolysis, the resulting reaction solution was evaporated under reduced pressure to remove water in the reaction solution. Filter to remove the sodium chloride generated by hydrolysis in the reaction solution, and use 10 mL of cold methanol solution to wash the filter residue, and further extract the product 3-methylthiopropanol in the filter residue. Finally, the mixed solution obtained after washing and the filt...

Embodiment 2

[0038] Table 2 is the influence of different amounts of reducing agent on the preparation of 3-methylthiopropanol from 3-methylthiopropanal (MMP). Add sodium borohydride (NaBH 4 ) into 30 mL of 3-methylthiopropanol solvent to obtain a suspension. Then, 10 g of 3-methylthiopropanal (MMP) was slowly added dropwise to the resulting suspension while controlling the temperature below 20°C. After the dropwise addition is completed, stir at room temperature, and after 3-12 hours, add hydrochloric acid (HCl) solution to the reaction solution for hydrolysis. After hydrolysis, the resulting reaction solution was evaporated under reduced pressure to remove water in the reaction solution. Filter to remove the sodium chloride generated by hydrolysis in the reaction solution, and use 10 mL of cold methanol solution to wash the filter residue, and further extract the product 3-methylthiopropanol in the filter residue. Finally, the mixed solution obtained after washing and the filtrate wer...

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Abstract

The invention provides a method for preparation of 3-methylthiopropanol from 3-methylthiopropanal by reduction reaction under a solvent or solvent-free condition. The invention further includes purification treatment on the reaction mixture, and the obtained product has purity higher than 99.0%. The preparation method uses a reactive solvent containing 3-methylthiopropanol component, and compared with other organic solvents can effectively increase the yield of 3-methylthiopropanol.

Description

technical field [0001] The invention relates to a preparation method of methylmercaptan, in particular to a method for preparing 3-methylthiopropanol from 3-methylthiopropanal. Background technique [0002] 3-Methylthiopropanol and its derivative compounds are the main aroma components in fermented foods, and it is also an important essence of various fruity, meaty, and wine flavors. At present, 3-methylthiopropanol is widely used in food, cosmetics, daily chemicals, pharmaceutical and tobacco industries. As a food flavor, 3-methylthiopropanol can not only make up the fragrance of food but also cover up the unpleasant smell by adding food additives. Therefore, for the food industry, 3-methylthiopropanol is a very important additive. Generally, propanol and methanethiol (MeSH) or chloropropanol and sodium thiol (MeSNa) are generally used in industrial production to prepare 3-methylthiopropanol. However, the preparation method is complex, low yield, high cost and unsustaina...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C319/20C07C323/12
CPCC07C319/20C07C323/12
Inventor 吉达尔·瓦伦汀布泰·朱利安
Owner BLUESTAR ADISSEO NANJING CO LTD
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