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Preparation of 4-alkyl cyclohexyl acetaldehyde

A technology of alkyl rings and alkyl groups, which is applied in the field of preparation of 4-alkylcyclohexylacetaldehyde, and can solve the problems of complex synthesis methods and low total yields

Inactive Publication Date: 2008-12-17
SHANGHAI CHEMSPEC CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In the prior art, the synthesis method of this type of compound is relatively complicated, for example, a 6-step synthesis route is used in the patent JP03068561, and the overall yield is low

Method used

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  • Preparation of 4-alkyl cyclohexyl acetaldehyde
  • Preparation of 4-alkyl cyclohexyl acetaldehyde
  • Preparation of 4-alkyl cyclohexyl acetaldehyde

Examples

Experimental program
Comparison scheme
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preparation example Construction

[0138] (2) The preparation method of the present invention can effectively avoid the generation of high-boiling point by-products, provide convenience for subsequent purification and making mixed crystals, improve the yield and purity of the final single crystal, and affect the electrical properties after the mixed crystals No adverse effects will be expected.

[0139] The above-mentioned synthetic method is only the synthetic route of some compounds of the present invention. According to the above-mentioned examples, those skilled in the art can synthesize other compounds of the present invention by adjusting different methods, or those skilled in the art can synthesize the compounds of the present invention according to the existing known techniques. compound. The synthesized compound can be further purified by column chromatography, high performance liquid chromatography or crystallization.

[0140] Synthetic chemical modification, protected functional group methodology (p...

Embodiment 1

[0144] Embodiment 1 prepares 4-n-propyl methoxy methylene cyclohexane

[0145] Add 50g (0.45mol) of tert-butanol methyl (0.45mol) and 200ml (0.18mol) of tetrahydrofuran into a 500ml four-necked reaction flask, cool to 0°C, and slowly add 148g (0.43mol) of methoxymethyltriphenylphosphorus chloride under stirring. , 20 minutes to complete the addition, heat preservation reaction for 1 hour after the addition, slowly add 50 g (0.36 mol) of 4-n-propyl cyclohexanone at 0 ° C, add and heat preservation reaction for 1 hour, pour into 400 ml of water, add 600 ml of toluene Extracted, washed with water until neutral, dried with anhydrous magnesium sulfate, and evaporated toluene to obtain 58 g of 4-n-propylmethoxymethylenecyclohexane with a content of 93.4% and a yield of 90%.

Embodiment 2～6

[0147] Carry out in the same manner as Example 1, except that reaction temperature, formula (I) compound: the molar ratio of catalyst A and formula (I): the molar ratio of base is shown in Table 1. Table 1 also shows the yield, purity and high boiler (ie bottom tar fraction) content of the compound of formula (II) in the obtained product.

[0148] Table 1

[0149] implement

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Abstract

The invention provides a preparation method of 4-alkyl cyclohexyl acetaldehyde, which comprises the following steps: the 4-alkyl cyclohexyl acetaldehyde is gained from 4-alkyl cyclohexanone and through steps including Wittig reaction, hydrolysis reaction, Wittig reaction and hydrolysis reaction. The method of the invention has advantages of short synthetic route, simple technology and mild conditions, and can gain the 4-alkyl cyclohexyl acetaldehyde with quite high yield.

Description

technical field [0001] The present invention relates to a kind of preparation method of the intermediate of liquid crystal material, be specifically related to the preparation method of 4-alkyl cyclohexyl acetaldehyde Background technique [0002] 1-Ethoxy-2,3-difluoro-4[2-alkylcyclohexyl]ethylbenzene is a new liquid crystal material suitable for polymeric polymer stable orientation technology and can take into account the optical performance of liquid crystal panels . And 4-alkyl cyclohexyl acetaldehyde is an important intermediate in the synthesis of this material, and this type of compound can be represented by the following chemical formula: [0003] [0004] In the prior art, the synthesis method of this type of compound is relatively complicated, for example, a 6-step synthesis route is used in the patent JP03068561, and the overall yield is low. [0005] In summary, this area lacks a preparation method of 4-alkylcyclohexylacetaldehyde. This method reacts with ind...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/11C07C45/37
Inventor 杨凯袁云龙
Owner SHANGHAI CHEMSPEC CORP