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Easter compounds and preparation method thereof

A technology of ester compounds and compounds, applied in the field of ester compounds and their preparation, can solve the problems of high toxicity of raw materials, complicated preparation process, environmental pollution, etc.

Active Publication Date: 2013-08-07
DONGYING ANNUOQI TEXTILE MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The technical problem to be solved by the present invention is to provide an ester compound and its preparation method in order to overcome the defects of the existing dyestuffs such as complex preparation process, high toxicity of raw materials, cumbersome post-processing operations, and serious environmental pollution.

Method used

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  • Easter compounds and preparation method thereof
  • Easter compounds and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0147] The preparation of embodiment 1 compound 6

[0148]

[0149] At room temperature, add 67 parts by weight of 30% sodium hydroxide aqueous solution into a three-necked flask, then add 47 parts by weight of phenol and 5 parts by weight of PEG-400 under stirring, stir evenly, and then use dropwise Slowly add 66 parts of heavy epichlorohydrin into the funnel dropwise for about 1-2 hours. After the dropwise addition, slowly raise the temperature to 50°C-55°C for reaction. After 3h-5h, the raw materials react completely, add 50mL of water to fully dissolve the solid, and then Stand for stratification, remove the water phase, add 100mL of water for washing, and adjust the pH to neutral with a small amount of dilute hydrochloric acid, stir well and then stand for stratification, collect the oil phase, and distill under reduced pressure to remove excess epichlorohydrin and water. 52 g of the compound of the following formula was obtained, the yield was 70.5%, and the HPLC pur...

Embodiment 2

[0150] Example 2 Compound 4 (R 1 for H, R 2 for H, R 3 for the preparation of ethyl)

[0151] Add 18 parts by weight of N-ethylaniline and 30 parts by weight of acetic acid into a three-necked flask, stir evenly and then slowly raise the temperature to 50°C, then slowly add 24 parts by weight of compound 6 dropwise from a constant pressure dropping funnel for about 3 hours ~ 4h, after the addition, keep it warm at 50°C for 3h ~ 4h to complete the reaction, and compound 4 (R 1 for H, R 2 for H, R 3 Ethyl) in acetic acid solution was directly used in the next reaction. Yield 97.3%, HPLC purity 92.4%, LC-MS (ESI): [M+H] + 272.2, [M+Na] + 294.2.

[0152]

Embodiment 3

[0153] Embodiment 3 ester compound 2-1 (R 1 for H, R 2 for H, R 3 is ethyl, R 4 for the preparation of methyl)

[0154] 29 parts of heavy compound 4 (R 1 for H, R 2 for H, R 3 Ethyl) into a three-necked flask, slowly warm up to 50°C, at this temperature, slowly add 13 parts of heavy acetic anhydride dropwise from a constant pressure dropping funnel, dropwise for about 2 hours, and keep warm at 50°C until the reaction of the raw materials is complete , to obtain ester compound 2-1 (R 1 for H, R 2 for H, R 3 is ethyl, R 4 Methyl) in acetic acid solution, yield 96.1%, HPLC purity 94.3%, LC-MS (ESI): [M+H] + 314.4, [M+Na] + 336.4.

[0155]

[0156] The ester compounds 2-1 to 2-12 were prepared according to the methods of Examples 1 to 3, and their relevant experimental data and structure identification data are shown in Table 1.

[0157] Table 1 Experimental data and structural identification data of compounds 2-1~2-12

[0158]

[0159]

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PUM

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Abstract

The invention discloses ester compounds and a preparation method thereof. The invention provides the ester compounds represented by a formula 2, wherein R1 is C1-4 alkoxy or hydrogen, R2 is C1-4 acylamino or hydrogen, R3 is C1-4 alkyl, and R4 is C1-4 alkyl. The preparation method of the ester compounds represented by the formula 2 has the step that: a compound 4 and anhydride represented by a formula 5 are subjected to an acylation reaction, such that the eater compound 2 is obtained.

Description

technical field [0001] The invention relates to an ester compound and a preparation method thereof. Background technique [0002] Disperse dyes are a kind of non-ionic dyes with simple structure and low water solubility, which mainly exist in the dispersed state of tiny particles in the dye bath. It came out as early as the early 1920s. It was mainly used in the dyeing of acetate fiber at that time, so it was also called acetate fiber dye. In recent years, with the rapid development of synthetic fibers, especially polyester fibers, disperse dyes have gradually become one of the fastest-growing dyes in modern times. At present, it is mainly used for dyeing and printing of polyester fiber, and it can also be used for dyeing of hydrophobic textile materials such as acetate fiber and polyamide fiber. With the improvement of people's living standards, consumers have higher and higher requirements for the performance of textiles. For example, dyed textiles are required to have h...

Claims

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Application Information

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IPC IPC(8): C09B29/09C09B29/085C07C219/06C07C213/06C07C233/43C07C231/12C07C217/30C07C213/04D06P1/18D06P1/19D06P3/54D06P3/85
Inventor 韩伟鹏赵敏
Owner DONGYING ANNUOQI TEXTILE MATERIALS
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