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1-isopropylcyclohexanol methyl propionate and preparation method thereof

A technology of alcohol methyl propionate and isopropyl cyclohexanol, which is applied in the field of synthesis of organic compounds, can solve the problems of many side reactions, low reaction yield, and inapplicability to industrial production, so as to improve yield and operate Simple process and good stability

Inactive Publication Date: 2015-03-04
上海博康睿玉贸易发展有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the substances disclosed in the prior art for producing photoresists are relatively single and limited, and in the synthesis process, there are often difficulties in purification, many side reactions, low reaction yield, low product purity, and are not suitable for large-scale industrialization. Production and other issues

Method used

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  • 1-isopropylcyclohexanol methyl propionate and preparation method thereof
  • 1-isopropylcyclohexanol methyl propionate and preparation method thereof
  • 1-isopropylcyclohexanol methyl propionate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0063] (1) The reaction equation is as follows:

[0064]

[0065] (2) Specific process steps:

[0066] Under the protection of nitrogen, add 245g of magnesium chips to 738.7g of tetrahydrofuran, add 1ml of 1,2-dibromoethane, and stir well. At room temperature (30 degrees), start to add 2-chloropropane (800g) in tetrahydrofuran (1023.5g) solution, after about 10% dropwise, stop the 2-chloropropane solution, and heat to 60 degrees, the reaction gradually starts, At this time, a large amount of heat is released, and the heat source needs to be removed, and the temperature is changed to a water bath to cool down. After keeping the reaction exothermic stable, continue to add (2-chloropropane) bromoethane solution dropwise to maintain a slight boiling (about 67 degrees), and finish dripping in 1.5 hours After dripping, keep stirring at this temperature for 2 hours (the solution is dark gray at this time).

[0067] Cool the reaction solution to 0-5 degrees, then add a solution of cyclohex...

Embodiment 2

[0074] (1) The reaction equation is as follows:

[0075]

[0076] (2) Specific process steps:

[0077] Add 1250g methacrylic acid and 1518g methacryloyl chloride to 8379g dichloromethane at room temperature, cool to -10-0 degrees, add 1575g triethylamine dropwise, control the internal temperature <0 degrees, about 45 minutes after dripping, take a sample (central control 1). The reaction mixture was poured into 10 kg of ice water, stirred for 30 minutes and then separated into layers. The upper aqueous phase was extracted with dichloromethane (3990g×1), the organic phases were combined, and the organic phase was washed with water (2000g×1) and rotated. Dry solvent (30 degrees), the obtained crude product is added with 1% (wt / wt) of phenothiazine and then subjected to vacuum distillation (oil pump, thorn-type fractionating column, fraction temperature 75-80 degrees, oil temperature 130 degrees) to obtain colorless Liquid 1340g (central control 2)

[0078] (3) The processing method o...

Embodiment 3

[0081] (1) The reaction equation is as follows:

[0082]

[0083] (2) Specific process steps:

[0084] Under the protection of nitrogen, add 712g of tetrahydrofuran to the reaction flask, cool to -25--15 degrees, then add 572g of n-butyl lithium (n-butyl lithium solution with a density of 0.65), and control the internal temperature to not exceed -15 degrees. , Add it in about 15 minutes. Then, after dissolving 216 g of 1-isopropylcyclohexanol in 445 g of tetrahydrofuran, slowly drip into the reaction flask, control the internal temperature not to exceed -20 degrees, and finish the drip in about 40 minutes. After dripping, the reaction flask was heated to 20-25 degrees and continued to stir for 1 hour, and then re-cooled to -5-0 degrees, 346g of methacrylic anhydride was dropped into the reaction flask, control the internal temperature not to exceed 0 degrees, about 40 minutes Finish dripping. Remove the ice bath, raise to room temperature (20-25 degrees) and continue to react fo...

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Abstract

The invention provides a 1-isopropylcyclohexanol methyl propionate. The 1-isopropylcyclohexanol methyl propionate is characterized by being represented by the following structural formula as shown in the specification. A preparation method comprises the following steps of reacting cyclohexanone and a Grignard reagent to obtain 1-isopropylcyclohexanol and reacting 1-isopropylcyclohexanol and methacrylic anhydride to generate 1-isopropylcyclohexanol methyl propionate. By providing a compound and a synthetic route thereof and optimizing and screening the synthetic method, the problems of low yield, complex reaction and high purification difficultly are overcome and a product having the advantages of high yield, simple treatment process and high purity is obtained.

Description

Technical field [0001] The invention relates to a method for synthesizing organic compounds, particularly 1-isopropylcyclohexanol methyl propionate and a preparation method thereof. Background technique [0002] Photoresist, also known as photoresist, refers to an etch-resistant thin film material whose solubility changes through ultraviolet light, electron beam, ion beam, X-ray, etc. irradiation or radiation. After exposure and development, the solubility is increased by positive photoresist, and the solubility is decreased by negative photoresist. According to the different exposure light source and radiation source, it is divided into ultraviolet photoresist (including ultraviolet positive and negative photoresist), deep ultraviolet photoresist, electron beam glue, X-ray glue, ion beam glue and so on. [0003] Photoresist is a key material required for the production of integrated circuits. It develops with the development of integrated circuits and is constantly updated. Acco...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C69/54C07C69/24C07C67/08
CPCC07C67/08C07C29/40C07C2601/14
Inventor 贺宝元傅志伟潘新刚
Owner 上海博康睿玉贸易发展有限公司
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