Preparation method for disperse red

A disperse red and compound technology, applied in chemical instruments and methods, organic dyes, azo dyes, etc., can solve problems such as affecting the synthesis of target products, low intermediate yields, and unfavorable industrial production, and achieve industrial operability. Strong, simple preparation, high product purity effect

Inactive Publication Date: 2013-02-13
江苏德旺数码科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The preparation process reported in the current market and literature, the yield of intermediates is not high, which affects the synthesis of the target product, resulting in higher costs, which is not conducive to industrial production

Method used

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  • Preparation method for disperse red
  • Preparation method for disperse red

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Experimental program
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Effect test

Embodiment 1

[0020] 1) Add 19.9g (0.18mol) of hydroquinone and 21.9g (0.144mol) of mandelic acid to the reactor in turn, start stirring, add 76.6g of sulfuric acid aqueous solution with a mass concentration of 75%, raise the temperature to 105°C, react for 25min, and perform HPLC It was detected that the reaction of mandelic acid was complete, cooled to 20°C, poured into ice water, stirred for 25 minutes, suction filtered, the filter cake was washed with ice water, dried in vacuo, and recrystallized with toluene to obtain 29.9 g of compound (III), with a yield of 91.4%, m.p. 158~159℃;

[0021] 2) Add 10.0g (0.044mol) of compound (III), 2000g of glacial acetic acid and 12g of phosphoric acid into the reactor, raise the temperature to 72°C, add 8.4g (0.055mol) of p-propoxymandelic acid, and control the temperature of the reaction system at 72 ℃, after the addition, keep stirring at 72℃ for 1.5h, HPLC detects that the compound (III) has reacted completely, cool to 0~5℃, filter with suction, w...

Embodiment 2

[0024] 1) Add 19.9g (0.18mol) of hydroquinone and 22.2g (0.146mol) of mandelic acid to the reactor in turn, start stirring, add 70g of sulfuric acid aqueous solution with a mass concentration of 80%, raise the temperature to 110°C, react for 20min, and detect by HPLC Mandelic acid was completely reacted, cooled to 20°C, poured into ice water, stirred for 25 min, filtered with suction, washed with ice water, dried in vacuo, recrystallized from toluene to obtain 30.1 g of compound (III), yield 92.1%, m.p.158 ~159°C;

[0025] 2) Add 10.0g (0.044mol) of compound (III), 2100g of glacial acetic acid and 11g of phosphoric acid into the reactor, raise the temperature to 75°C, add 10.1g (0.066mol) of p-propoxymandelic acid, and control the temperature of the reaction system at 75 °C, after the addition, keep stirring at 75 °C for 1.3 h, HPLC detects that the compound (III) has reacted completely, cool to 0~5 °C, filter with suction, wash the filter cake with ethanol alcohol at 0~5 °C, ...

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Abstract

The invention discloses a preparation method for disperse red, which comprises the following steps: hydroquinone is reacted with mandelic acid to obtain an intermediate compound (III); the compound (III) is further reacted with propoxy mandelic acid in presence of phosphoric acid to obtain an intermediate compound (II); and the intermediate compound (II) is oxidized by chloranil to obtain the target product. The process route disclosed by the invention is simple in preparation and strong in industrial operability; the yield of the compound (III) preparation step is over 91%; the yield of the compound (II) preparation step is over 71%; the yield in the preparation process of the target product compound (I) is over 98%; and the final product purity is high and is above 99.8%.

Description

technical field [0001] The invention relates to the field of preparation of disperse dyes, in particular to a preparation method of disperse red. Background technique [0002] Benzodifuranone disperse dyes have been widely valued for their bright color, high color strength and good dyeing performance, especially in the application of polyester microfibers. Disperse Red 356 is the largest variety of benzodifuranone disperse dyes. Its chemical name is 3-phenyl-7-(4-propoxyphenyl)-benzodifuran-2,6-dione. The structural formula is: [0003] [0004] In the preparation process reported in the market and literature, the intermediate yield is not high, which affects the synthesis of the target product, resulting in higher cost and unfavorable for industrial production. Contents of the invention [0005] The technical problem to be solved by the present invention is to provide a preparation method of disperse red with simple process and high yield. [0006] For solving the p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09B57/00
Inventor 杨泽辉何明华钱益民黄祥保
Owner 江苏德旺数码科技有限公司
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