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Method for preparing 2-alkyl carboxylic acid

A technology of alkyl carboxylic acid and alkyl group, applied in the field of preparing 2-alkyl carboxylic acid, can solve the problems of expensive raw materials, high cost and rare, and achieve the effects of convenient operation, less by-products and high production process yield

Inactive Publication Date: 2010-03-10
上海立科化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The raw materials of the above-mentioned methods are relatively expensive and rare, and the relative cost of the reagents used is relatively high

Method used

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  • Method for preparing 2-alkyl carboxylic acid
  • Method for preparing 2-alkyl carboxylic acid
  • Method for preparing 2-alkyl carboxylic acid

Examples

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Embodiment 1

[0027] A kind of method for preparing 2-alkyl carboxylic acid, when R 1 is n-hexyl, R 2 is methyl, R 3 When being a methyl group, the general reaction formula is as follows:

[0028]

[0029] The preparation method comprises the following steps:

[0030] The first step: the synthesis of 3-hydroxyl-1-nonene (4):

[0031] Add 3g (0.125mol) of magnesium chips to a 250ml four-necked bottle, add 20ml of tetrahydrofuran (THF), stir under nitrogen protection, add a small grain of iodine (40mg) and 0.5ml of 1,2-dibromoethane as the initiator, heat, System initiation, reaction at 60°C, 13.7 g (0.113 mol) of n-chlorohexane (1) was slowly added dropwise, and the addition was completed in 50 minutes, and the reaction was carried out at 45°C. After 2 hours, GC tracking showed that the reaction of raw materials was complete. Transfer the reaction solution into a 250ml dropping funnel, slowly dropwise add acrolein (3) 9.5g, (0.170mol) and THF (50ml) mixture, control the temperature at...

Embodiment 2

[0054] A kind of method for preparing 2-alkyl carboxylic acid, when R 1 is n-propyl, R 2 is ethyl, R 3 When being a methyl group, the general reaction formula is as follows:

[0055]

[0056] The preparation method comprises the following steps:

[0057] The first step: the synthesis of 3-hydroxyl-1-hexene (11):

[0058] Add 5g (0.208mol) magnesium chips to a 250ml four-necked bottle, add 30ml THF, stir under nitrogen protection, add a small grain of iodine (about 40mg) and 0.5ml of 1,2-dibromoethane as the initiator, heat, and the system initiates , reacted at 60°C, slowly added 14.9g (0.189mol) of n-chloropropane (9) dropwise, and the addition was completed in 50 minutes. After reacting at 40°C for 2 hours, GC tracking showed that the reaction of the raw materials was completed. The reaction solution was slowly added dropwise to a mixture of 15.9 g (0.283 mol) of acrolein (3) and THF (50 ml), the temperature was controlled at 5-10°C, the dropwise addition was complete...

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Abstract

The invention relates to the fields of chemical industry and pharmacy and provides a method for preparing 2-alkyl carboxylic acid. The method comprises the following reaction steps: step one: leadingalkyl halide R<1>-X and metal magnesium to react so as to prepare a Grignard reagent, leading the Grignard reagent and acraldehyde to react so as to prepare an enol intermediate; step two: leading theenol intermediate and ortho ester to react so as to prepare 2-alkyl-4-enes-alkanoate after rearrangement; step three: reducing the 2-alkyl-4-enes-alkanoate by palladium-charcoal so as to obtain 2-alkyl-alkanoate; step four: adding alkali in the 2-alkyl-alkanoate to carry out hydrolysis and adding acid in the 2-alkyl-alkanoate to carry out acidification so as to obtain corresponding 2-alkyl carboxylic acid, wherein in the alkyl halide, R<1> is straight chain or branch chain alkyl of C1 to C10, X is C1, Br or I; and in the ortho ester, R<2> and R<3> are straight chain or branch chain alkyl of C1 to C3. When the method is applied to the synthesis of 2-alkyl carboxylic acid, the yield of the obtained product is high, the operation step is simple and the cost is low.

Description

technical field [0001] The invention relates to the fields of chemical industry and pharmacy, in particular to a method for preparing 2-alkyl carboxylic acid. Background technique [0002] Pine trees are important forest resources in my country. For a long time, with the continuous increase of the plantation area and the gradual deterioration of the forest ecological environment, the pine leaf bee pests often burst into disasters. According to the survey in the past ten years, there are more than 10 kinds of pine sawflies that occur in large areas in my country, which pose a serious threat to the survival and development of local pine plantations and cause huge economic losses. One of the important forest pests. [0003] In the past 20 years, people have been committed to using pheromones of pests to selectively control them, fundamentally overcoming the fatal defects of traditional pesticides that destroy ecological balance and pollute the environment. In the 1960s, Coppe...

Claims

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Application Information

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IPC IPC(8): C07C53/128C07C51/09
Inventor 朱高军曾志宏张芳江薛涛
Owner 上海立科化学科技有限公司
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