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Method for preparing 2,6-dimethyl-2-heptanol

A technology of dimethyl and heptanol, applied in 2 fields, can solve the problems of difficulty in ensuring product yield and operational safety, inconspicuous initiation, long initiation time, etc., and achieves high product yield, fast initiation speed, and easy storage. Effect

Active Publication Date: 2008-02-20
格林生物科技股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, such initiators are often highly toxic, and the triggering is not obvious or the triggering time is too long when it is amplified in production
Methyl chloride and methyl bromide, the main raw materials for the preparation of methylmagnesium chloride and methylmagnesium bromide, are gases at normal temperature and pressure, which have certain toxicity and danger. It is difficult to guarantee the product yield and operational safety by using the above initiators.

Method used

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  • Method for preparing 2,6-dimethyl-2-heptanol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Preparation of benzyl magnesium chloride: prepare 12.7 g (0.1 mol) of benzyl chloride and 60 mL of tetrahydrofuran, and stir for 5 min for use. In a clean and dry 250mL four-necked flask, add 2.4g (0.1mol) of freshly treated magnesium powder, 15mL of tetrahydrofuran, and 15mL of toluene. After stirring for 5min, the temperature is slowly raised to 60°C. After stabilization, 5% of the prepared solution is slowly added dropwise. The mixture of benzyl chloride and tetrahydrofuran, the reaction exotherm is obvious, and the reaction has been initiated when the temperature no longer rises. Continue to add the remaining mixture of benzyl chloride and tetrahydrofuran dropwise, the reaction is obviously exothermic, keep cooling during the process, the reaction temperature is controlled at 10~60°C, the dripping is completed in about 6~8 hours, and the reaction is completed after continuing the reaction for 3 hours. The prepared initiator was stored in a sealed reagent bottle unti...

Embodiment 2

[0027] Preparation of benzyl magnesium bromide: prepare 17.1 g (0.1 mol) of benzyl bromide and 100 mL of tetrahydrofuran, and stir for 5 min for use. In a clean and dry 250mL four-necked flask, add 2.4g (0.1mol) of freshly treated magnesium powder, 30mL of tetrahydrofuran, and 10mL of toluene. After stirring for 5min, the temperature is slowly raised to 60°C. After stabilization, 5% of the prepared solution is slowly added dropwise. The mixture of benzyl bromide and tetrahydrofuran, the reaction exotherm is obvious, and the reaction has been initiated when the temperature no longer rises. Continue to add the remaining mixture of benzyl bromide and tetrahydrofuran dropwise, the reaction is obviously exothermic, keep cooling during the process, the reaction temperature is controlled at 10~60℃, about 6~10h is the end of dripping, and the reaction is completed after continuing the reaction for 3h. The prepared initiator was stored in a sealed reagent bottle until use.

Embodiment 3

[0029] The preparation of 2,6-dimethyl-5-hepten-2-ol: in a clean and dry 1000mL four-necked flask, add 24g (1mol) of freshly treated magnesium powder, 240mL of tetrahydrofuran, and after stirring at room temperature for 5min, Then add 10 g of prepared benzyl magnesium bromide and 4 g of benzyl bromide, and the reaction is quickly initiated under stirring. After the initiation is complete, slowly pass into methyl chloride, and react in a boiling state. The magnesium powder disappears completely in about 3 to 6 hours. Continue React for 1h. Place the prepared four-necked flask of methylmagnesium chloride Grignard reagent in the cooling system, start stirring, and control the internal temperature to slowly add 126g (1mol) 6-methyl-5-heptene-2- Ketone, the dropwise addition time is about 2~5h, continue to react at room temperature for 1h after the dropwise addition, add 200mL toluene after the reaction, recover tetrahydrofuran at normal pressure, slowly add 250g 20% ​​acetic acid ...

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Abstract

The invention discloses a preparation method of an organism in chemical industry technical field, in particular to the preparation method of a 2, 6-Dimethyl-2-Heptanol. The invention is that: firstly methylic Grignard reagent is prepared through taking Benzyl magnesium Chloride or Benzyl magnesium Bromide as an initiator, then is carried out the Grignard reaction with 2-Methyl-2-Hepten-6-Ketone, and finally is catalyzed and hydrogenated to synthesize 2,6-Dimethyl-2-Heptanol. The initiator prepared by the invention has the advantages of relatively stable property, easy preservation, higher initiating speed compared with commonly used initiator, strong universality, low dosage, convenient storage and low toxicity, etc. The initiator is especially suitable for preparing Grignard Reagent in mass production. The product prepared by the invention has better security and higher yield. The prepared product can be widely used in essence prescription of daily chemistry.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and relates to a preparation method of 2,6-dimethyl-2-heptanol. technical background [0002] 2,6-Dimethyl-2-heptanol (2,6-Dimethyl-2-heptanol) has fresh lily-of-the-valley and citrus notes, and can be used in perfume formulations. [0003] The main methods for preparing 2,6-dimethyl-2-heptanol are 6-methyl-5-hepten-2-one and several methyl magnesium chloride or methyl magnesium bromide or methyl magnesium iodide. Grignard reagent reaction, and catalytic hydrogenation; or use 2-methyl-6-heptanone as raw material to carry out Grignard reaction. [0004] [0005] Halogenated hydrocarbons react with metal magnesium in anhydrous ether or tetrahydrofuran to generate alkyl magnesium halide RMgX. This organomagnesium compound is called Grignard Reagent. Grignard reagents can undergo addition reactions with aldehydes, ketones and other compounds, and generate alcohols after hydrolysis. Suc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C31/125C07C29/17C07B49/00
Inventor 林传明叶剑飞尤坚萍白传伟胡建良陆文聪
Owner 格林生物科技股份有限公司
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