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Method for preparing disperse red SBWF

A technology of disperse red and tetrahydrofuran, applied in chemical instruments and methods, azo dyes, organic dyes, etc., can solve the problems of strict operational safety technical requirements, difficult treatment of "three wastes", long process route, etc., and achieve easy control of reactions , Exempt the risk of high-risk operation, the effect of high oxidation efficiency

Inactive Publication Date: 2020-02-14
JIANGSU OCEAN UNIV +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Patent CN104725391 uses tetrahydrofurfuryl alcohol and p-toluenesulfonyl chloride as raw materials, and obtains SBWF through steps such as acylation, condensation, cyanation, and chloranil oxidation. Large, high operating requirements, difficult to deal with "three wastes"
Patent CN108410204 uses oxalyl chloride monoalkyl ester as raw material to prepare the target product SBWF through multiple steps such as Friedel-Crafts reaction, hydrogenation reaction, condensation reaction, oxidation reaction, etc. The process route is long, the process adopts hydrogenation process, and the reaction pressure is relatively high , strict requirements on operational safety technology

Method used

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  • Method for preparing disperse red SBWF
  • Method for preparing disperse red SBWF

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] 1) Add 20.5g of 4-(tetrahydrofuran-2-methoxy)-benzaldehyde, 2g of benzyltriethylammonium chloride, and 49g of chloroform into a three-necked flask in sequence, heat in a water bath, and stir vigorously. The temperature was raised to 50° C., and 33 g of 40% NaOH solution was added dropwise at a rate of 20 seconds per drop. After the dropwise addition was completed, the reaction was continued for 3 hours while maintaining the temperature at 60°C. Follow up the reaction with high performance liquid chromatography, with the content of 4-(tetrahydrofuran-2-methoxyl)-benzaldehyde being lower than 1% as the end point of the reaction, after the reaction is completed, the temperature is naturally lowered, and an appropriate amount of water and chloroform is added to stir, and left to stand for 30 minutes, layered. Separate the organic layer, and use a rotary evaporator to recover chloroform from the organic layer; add 30% hydrochloric acid to the aqueous layer to acidify to pH ...

Embodiment 2

[0019] 1) Add 20.5g of 4-(tetrahydrofuran-2-methoxy)-benzaldehyde, 2.5g of hexadecyltrimethylammonium bromide, and 52g of chloroform into a three-necked flask in sequence, heat in a water bath, and stir vigorously. The temperature was raised to 55° C., and 40 g of 40% NaOH solution was added dropwise at a rate of 20 seconds per drop. After the dropwise addition was completed, the reaction was continued for 3 hours while maintaining the temperature at 60°C. Follow up the reaction with high performance liquid chromatography, with the content of 4-(tetrahydrofuran-2-methoxyl)-benzaldehyde being lower than 1% as the end point of the reaction, after the reaction is completed, the temperature is naturally lowered, and an appropriate amount of water and chloroform is added to stir, and left to stand for 30 minutes, layered. Separate the organic layer, and use a rotary evaporator to recover chloroform from the organic layer; add 30% hydrochloric acid to the aqueous layer to acidify t...

Embodiment 3

[0022] 1) Add 20.5g of 4-(tetrahydrofuran-2-methoxy)-benzaldehyde, 2g of benzyltriethylammonium chloride, and 52g of chloroform into a three-necked flask in sequence, heat in a water bath, and stir vigorously. The temperature was raised to 53° C., and 39 g of 40% NaOH solution was added dropwise at a rate of 20 seconds per drop. After the dropwise addition was completed, the reaction was continued for 3 hours while maintaining the temperature at 60°C. Follow up the reaction with high performance liquid chromatography, with the content of 4-(tetrahydrofuran-2-methoxyl)-benzaldehyde being lower than 1% as the end point of the reaction, after the reaction is completed, the temperature is naturally lowered, and an appropriate amount of water and chloroform is added to stir, and left to stand for 30 minutes, layered. Separate the organic layer, and use a rotary evaporator to recover chloroform from the organic layer; add 30% hydrochloric acid to the aqueous layer to acidify to pH ...

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Abstract

The invention relates to a preparation method of disperse red SBWF. The preparation method comprises the following specific steps: by using 4-(tetrahydrofuran-2-methoxy)-benzaldehyde and trichloromethane as raw materials, carrying out carbene reaction under the action of a phase transfer catalyst to prepare intermediate 4-(tetrahydrofuran-2-methoxy) mandelic acid; and carrying out condensation andoxidation of 4-(tetrahydrofuran-2-methoxy) mandelic acid and 5-hydroxy-3-phenyl-3H-benzofuran-2-one to prepare the target product 3-phenyl-7-(4-(tetrahydrofuran-2-methoxy) phenyl)-benzodifuran-2, 6-dione. The preparation method has the advantages of simplicity in operation, mild reaction conditions, environmental friendliness and the like, and has good industrial application value.

Description

technical field [0001] The invention relates to a preparation method of disperse red, in particular to a preparation method of disperse red SBWF, belonging to the technical field of chemical dye manufacture. Background technique [0002] Disperse Red SBWF, CAS: 134724-55-3, chemical name 3-phenyl-7-(4-(tetrahydrofuran-2-methoxy)phenyl)-benzodifuran-2,6-dione, It is a new variety of benzodifuranone disperse dyes. It has bright color and high color development strength. It is especially used on ultrafine polyester fibers and shows better coloring performance than other benzodifuranone dyes. The structural formula of disperse red SBWF is: [0003] [0004] Patent CN104725391 uses tetrahydrofurfuryl alcohol and p-toluenesulfonyl chloride as raw materials, and obtains SBWF through steps such as acylation, condensation, cyanation, and chloranil oxidation. Large, high operating requirements, difficult to deal with "three wastes". Patent CN108410204 uses oxalyl chloride monoal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B57/00C07D493/04
CPCC07D493/04C09B57/00
Inventor 许前会费学文姚邵伟赵剑桥杨辉郑建范晓楠古佳敏张浩桢张翔智
Owner JIANGSU OCEAN UNIV
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