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ChemicalBook CAS DataBase List Solvent Violet 13
81-48-1

Solvent Violet 13 synthesis

8synthesis methods
1,4-Dihydroxyanthracene-9,10-dione Or Anthracene-1,4,9,10-tetraol Or 1-Bromo-4-hydroxyanthraquinone Or 1-Chloro-4-hydroxyanthracene-9,10-dione and p-Methylaniline reaction.
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Yield:81-48-1 91.2%

Reaction Conditions:

with N-n-butyl-N'-ethylimidazolium chloride at 80 - 100;Large scale;Temperature;

Steps:

1.b; 1.c; 2-9; 1-2

(b) The ionic liquid is heated to 80 ° C, and then added to the high-pressure reaction vessel.820 kg of 1,4-dihydroxyanthraquinone, 142 kg of 1,4-dihydroxyanthraquinone leuco, and 430 kg of p-methylaniline, the reaction mixture was heated to 100 ° C to obtain a first mixed solution;(c) The first mixed solution is cooled to 45 ° C, the valve of the high-pressure reaction vessel is opened, and the material is discharged into a filter tank, and suction filtration is performed to obtain a filter cake and a filtrate. The filter cake is washed with hot water having a temperature of 95 ° C to obtain a foaming solution. The washing liquid and the filtrate are combined and distilled to obtain a second mixed solution; the washed cake is then post-processed, and the cake is washed with hot water at 90 ° C to neutrality, and then dried,Smash,1189 kg of finished product of solvent violet 13 was obtained in a package; the yield was 90.2%, the HPLC content was 95.63%, △ E 0.316, △ C 0.207 was bright, and the pressure value was 0.34.;This embodiment provides a method for synthesizing low-toxicity, low-toxicity and environmental-friendly solvent violet 13. It is basically the same as in Example 1. The difference is that 534 kg of ethyl chloride is added, and the solvent violet 13 is finally dried, crushed, and packaged. The finished product is 1202 kg; the yield is 91.2%, the HPLC content is 95.47%, △ E is 0.457, △ C is 0.318, and the pressure value is 0.37.

References:

CN110591407,2019,A Location in patent:Paragraph 0028; 0031-0052

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