81-42-5Relevant articles and documents
Environment-friendly and energy-saving process for synthesizing 1, 4-diamino-2, 3-dichloroanthraquinone
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Paragraph 0008-0009; 0019-0022, (2021/07/14)
The invention relates to the technical field of dye intermediates, in particular to a process for synthesizing 1, 4-diamino-2, 3-dichloroanthraquinone. The process comprises the following steps: adding a certain amount of chlorobenzene serving as a solvent into a reaction container, adding a certain amount of 1, 4-diaminoanthraquinone leuco body and zinc peroxide serving as a catalyst after the moisture is detected to be qualified, heating to 40-50 DEG C, and stirring and preserving heat for 10-20 minutes; stirring and dropwise adding quantitative sulfuryl chloride under the condition of 40-50 DEG C, and preserving heat for 10-60 minutes under the condition after dropwise adding is finished; after the reaction is completed, performing vacuum pumping for 30-60 minutes, and adding sodium carbonate to adjust the pH value of the reaction liquid to be nearly neutral; and performing water vapor distillation to recover the solvent, and filtering and washing the material to obtain the product. According to the synthesis process of the 1, 4-diamino-2, 3-dichloroanthraquinone provided by the invention, the catalyst zinc peroxide is added, so that the reaction temperature can be reduced, the reaction time can be shortened, the dosage of the sulfuryl chloride can be reduced, and the synthesis process has positive significance on reducing the cost and reducing the environmental protection pressure.
Refining process of 1,4-diamino-2,3-dichloroanthraquinone
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Paragraph 0009; 0010, (2019/01/08)
The invention discloses a refining process of 1,4-diamino-2,3-dichloroanthraquinone, belonging to the field of organic synthesis. The process comprises the steps of adding a 1,4-diamino-anthraquinoneleuco body into a container, dropwise adding chlorosulfuric acid at a temperature controlled at 35-40 DEG C in the presence of anhydrous nitrobenzene or o-dichlorobenzene as a solvent and azodiisobutyronitrile as a catalyst, holding the temperature at 50+/-5 DEG C for over 5 hours, pouring into 350-450 parts of water, adding a surfactant, neutralizing to be neutral with sodium carbonate, steam distilling the solvent reheating, filtering, washing with 80-DEG C hot water until the water is colorless and the pH is nearly neutral, discharging, and drying, so as to obtain 1,4-diamino-2,3-dichloroanthraquinone. The internal standard content of the refined 1,4-diamino-2,3-dichloroanthraquinone product can be increased by 2.5%-3.5%.
REACTION OF BORATE COMPLEXES OF 1,4-DIAMINO- AND 1-AMINO-4-HYDROXYANTHRAQUINONES WITH THE ANIONS OF CH ACIDS
Gorelik, M. V.,Mishina, E. V.
, p. 1892 - 1899 (2007/10/02)
The reaction of the diboroacetates of 1,4-diamino- and 1-amino-4-hydroxyanthraquinones with CH acids in an aprotic polar solvent in the presence of a base leads to the angular 5-amino- and 5-hydroxynaphtoindole-6,11-diones respectively.In the reaction of the diboroacetate of 2,3-dichloro-1,4-diaminoanthraquinone with dibenzoylmethane the main reaction product is the linear 4,11-diaminoanthrafuran-5,10-dione.