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Preparation method of 2-dimethyl-2-octanol

A technology of dimethyl and octanol, which is applied in the chemical industry, can solve the problems of long initiation time, inconspicuous initiation, and inconvenient production, and achieve the effects of fast initiation, high product yield, and convenient storage

Inactive Publication Date: 2013-04-24
HUAIAN WAN BANG SPICE IND CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this type of initiator is often highly toxic, and it is enlarged to the point where the initiation is not obvious or the initiation time is too long. In addition, in continuous production, each batch of production needs to make and put the initiator separately, which brings great inconvenience to production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Preparation of methylmagnesium chloride (initiator): Prepare 50 g (1 mol) of methyl chloride for use. Add 24 g (1 mol) of freshly treated magnesium powder, 260 g of tetrahydrofuran, and 0.3 g of iodine into a clean and dry 500 mL four-neck flask. After stirring for 5 min, slowly raise the temperature to 60 °C, and slowly add 4% chlorine When methane was added dropwise below the THF liquid level, the reaction exothermic was obvious, and when the temperature stopped rising, it indicated that the reaction had started. Continue to add the remaining methyl chloride dropwise below the tetrahydrofuran liquid level, the reaction is obviously exothermic, keep cooling during the process, the reaction temperature is controlled at 20°C, the drop is completed in about 3 hours, and the reaction is completed after continuing the reaction for 3 hours. Store the prepared initiator in a sealed reagent bottle for later use.

Embodiment 2

[0029] Preparation of methylmagnesium bromide (initiator): Prepare 95 g (1 mol) of methyl bromide for use. Add 24 g (1 mol) of freshly treated magnesium powder, 260 g of tetrahydrofuran, and 0.4 g of iodine into a clean and dry 500 mL four-neck flask. After stirring for 5 min, slowly raise the temperature to 60 °C, and slowly add 4% chlorine When methane was added dropwise below the THF liquid level, the reaction exothermic was obvious, and when the temperature stopped rising, it indicated that the reaction had started. Continue to add the remaining methyl chloride dropwise below the tetrahydrofuran liquid level, the reaction is obviously exothermic, keep cooling during the process, the reaction temperature is controlled at 20°C, the drop is completed in about 3 hours, and the reaction is completed after continuing the reaction for 3 hours. Store the prepared initiator in a sealed reagent bottle for later use.

Embodiment 3

[0031] Preparation of 2-dimethyl-2-octanol: Add 24 g (1 mol) of freshly treated magnesium powder and 240 g of tetrahydrofuran into a clean and dry 1000 mL four-neck flask, stir at room temperature for 5 min, and then Add 15g of the methylmagnesium chloride initiator prepared in Example 1, and the reaction will start rapidly under stirring. After the initiation is complete, slowly feed in methyl chloride to below the THF liquid level, and react in a boiling state. The magnesium powder will disappear completely in about 3 to 5 hours. , continue to react for 1 h. Place the prepared four-necked bottle of methylmagnesium chloride Grignard reagent in the cooling system, start stirring, and slowly add 128.2g (1 mol) of 2-octanone dropwise under the control of the internal temperature at 30-40°C, and the dropping time is about 2 ~5 h, continue to react at room temperature for 1 h after the dropwise addition, recover tetrahydrofuran under normal pressure, slowly add 250 g of 20% ac...

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PUM

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Abstract

The invention discloses a preparation method of 2-dimethyl-2-octanol. Methyl Grignard reagent is prepared by using methyl magnesium chloride or methyl magnesium bromide as an initiator. The 2-dimethyl-2-octanol is prepared by carrying out reaction of the methyl Grignard reagent and 2-octanone. The preparation method of the 2-dimethyl-2-octanol is suitable for continuous production, iodine is used for initiation for the first time, halogenated methane liquid state is added in the iodine in a dropwise manner to prepare an methyl magnesium chloride initiator and an methyl magnesium bromide initiator, and the methyl Grignard reagent produced in the previous production is completely adopted as the initiator in subsequent production to carry out the continuous production. The properties of the initiators of the preparation method are relatively stable. The initiator is easy to store, compared with a common initiator, the initiator has the advantages of being fast in initiation speed, strong in generality, low in usage, convenient to store and low in toxicity and the like, and is especially suitable for the preparation for the Grignard reagent in mass production. According to the preparation method of the 2-dimethyl-2-octanol, preparation safety is good, and production yield is high.

Description

Technical field [0001] The present invention is a chemical technology field, which involves a method of preparation of 2 -two -foundation, one 2, and meterol. Background technique [0002] 2 -two -foundation, one 2, one 2 and one (Dimethylhexylcarbinol) has a soft floral and green wood aroma, which can be used in the daily fragrance. [0003] Halogenic hydrocarbon is used to generate alkyl -backed magnesium RMGX in the role of hydrogen ether or tetrahydrofuu. This organic magnesium compound is called Grignard Reagent.The grid reagent can react with the aldehyde, ketone and other compounds. After hydrolyzed, alcohol is generated. Such reactions are called Gridnard Reaction. [0004] The key to preparing a reagent is whether the reaction can be proceeded smoothly, and the process is affected by many factors. During the experiment, due to the lack of lively marine hydrocarbons, the difficulty of removing the outer oxide of the magnesium powder, the trace water in the reagent or devi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/125C07C29/40
Inventor 邵建伟
Owner HUAIAN WAN BANG SPICE IND CO LTD
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