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1-methyl-cyclopentanol-acrylate and preparation method thereof

A technology of methyl cyclopentanol and acrylate, applied in the preparation of carboxylic acid halide, organic chemistry, etc., can solve the problems of low reaction yield, many side reactions, unsuitable for industrial production, etc., and achieves simple operation process and method. Simple and stable effect

Inactive Publication Date: 2015-03-25
上海博康精细化工有限公司
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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-methyl-cyclopentanol-acrylate and preparation method thereof
  • 1-methyl-cyclopentanol-acrylate and preparation method thereof
  • 1-methyl-cyclopentanol-acrylate and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] (1), the reaction equation is as follows:

[0051]

[0052] (2), specific process steps:

[0053] Into a 10L four-necked reaction flask, 4L of tetrahydrofuran and 482g of magnesium chips were added under nitrogen protection. At room temperature (8°C), 3363g of methyl bromide THF solution with a mass concentration of 61.8% was added dropwise, stirred to initiate, and the temperature was controlled to A , while cooling down naturally (from 65°C to 10°C), the solution becomes very viscous, (center control 1).

[0054]Slowly pour the reaction mixture into 5Kg (or 4kg, 5.5kg, 6kg or 6.5kg) of ice under stirring, then directly pour 1.6L concentrated HCl into the above reaction mixture under stirring, pH4 Dry, filter, and remove THF and DCM by rotary evaporation to obtain 1.9Kg of crude product (in-control 2).

[0055] Water pump vacuum distillation, external temperature 80-90°C, front fraction 41-49°C, 95g, (in-control 3). The external temperature is 90-95°C, the main fr...

Embodiment 2

[0061] (1), the reaction equation is as follows:

[0062]

[0063] (2), specific process steps:

[0064] Add 451g of A, 815g of acryloyl chloride, 3L of DCM, 9.0g (or 1.0g, 5.0g, 11.0g, 15g) of phenothiazine into a 10L four-neck flask, and cool to -10°C. 1002 g of triethylamine was added dropwise within 2 hours, solids were precipitated, and the reaction solution turned yellowish brown, and the color continued to deepen. The control temperature is less than 10°C. After the addition, react at room temperature (10° C.) for 1.5 h (in-control 1). Add 3L (or 2L, 3.5L, 4L) of saturated NaCl solution, separate the layers, extract the aqueous phase with (1.2L×3 times) DCM, combine the organic phases, and wash with (2L×2 times) saturated NaCl solution, without Dry over sodium sulfate, filter, and remove the solvent by rotary evaporation.

[0065] The crude products of the two batches of reactions were combined to a total of 2.4Kg, 2g (or 1.0g, 1.2, 0.7g, 0.1g) of p-tert-butylcat...

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Abstract

The invention provides a compound 1-methyl-cyclopentanol-acrylate. The compound 1-methyl-cyclopentanol-acrylate is characterized by being shown in a structural formula in the specification. The preparation method comprises the following steps: reacting a grignard reagent with cyclopentanone to generate 1-methyl cyclopentanol, and then reacting with acryloyl chloride, so as to generate 1-methyl-cyclopentanol-acrylate. Through providing a compound and a synthetic route thereof, and optimizing and screening the synthesis method, the problems of low productive rate, complicated reaction, high purification difficulty and the like are overcome; and the product which is high in productive rate, simple in processing process and high in purity is obtained.

Description

technical field [0001] The invention relates to a method for synthesizing organic compounds, in particular to 1-methyl-cyclopentanol-acrylate and a preparation method thereof. Background technique [0002] Photoresist, also known as photoresist, refers to an etching-resistant film material whose solubility changes through irradiation or radiation of ultraviolet light, electron beams, ion beams, X-rays, etc. Positive-type photoresists whose solubility increases through exposure and development, and negative-type photoresists whose solubility decreases. According to the different exposure light source and radiation source, it is divided into UV photoresist (including UV positive and negative photoresist), deep UV photoresist, electron beam glue, X-ray glue, ion beam glue, etc. [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. According to Moore's Law: t...

Claims

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Application Information

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IPC IPC(8): C07C67/14C07C69/54
CPCC07C67/14C07C2601/08
Inventor 贺宝元傅志伟潘新刚
Owner 上海博康精细化工有限公司
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