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Method for preparing vat golden yellow RK through oxidative bromination

A golden and RK technology, which is applied in the field of oxidative bromination to prepare reduced golden RK, can solve the problems of large environmental pollution, large risk factors, and non-conformity to greening, and achieve good selectivity, high atom utilization, and easy control of the reaction Effect

Inactive Publication Date: 2016-05-04
SINOPHARM CHEM REAGENT
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, during the reaction, controlled fuming sulfuric acid is used as a solvent, sodium nitrite and iodine are used as a catalyst, and liquid bromine is used as a bromination reagent. Bromination is carried out at 85-90 ° C. After the reaction, a large amount of waste acid is produced, which is a risk factor in the operation process. Large, large pollution to the environment, does not meet the requirements of modern chemical greening

Method used

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  • Method for preparing vat golden yellow RK through oxidative bromination
  • Method for preparing vat golden yellow RK through oxidative bromination

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Experimental program
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Effect test

Embodiment 1

[0019] Add 33.2g (0.1mol) reduced yellow GOK and 18.8g (0.2mol) urea peroxide into the reaction bottle, then add 200mL chloroform as solvent, heat to reflux under stirring, irradiate with 200W incandescent lamp, add 40% hydrogen dropwise 44.5 g (0.22 mol) of bromic acid, continue the reflux reaction for 2 h after the dropwise addition. After the reaction was completed, the reaction product reduced golden RK was directly filtered out after cooling, the filter cake was fully washed with chloroform and then dried to obtain the finished product, which was weighed to obtain 46.8 g, with a yield of 95.5%.

Embodiment 2

[0021] Add 33.2g (0.1mol) of reduced yellow GOK and 19.8g (0.21mol) of urea peroxide into the reaction flask, then add 200mL of 1,2-dichloroethane as a solvent, heat to reflux under stirring, and irradiate with a 200W incandescent lamp , 46.7 g (0.23 mol) of 40% hydrobromic acid was added dropwise, and the reflux reaction was continued for 3 h after the dropwise addition. After the reaction was completed, the reaction product reduced golden RK was directly filtered out after cooling, and the filter cake was fully washed with 1,2-dichloroethane and then dried to obtain the finished product, which was 45.4 g by weight, with a yield of 92.7%.

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Abstract

The invention relates to a method for preparing vat golden yellow RK through oxidative bromination, and belongs to the technical field of organic synthesis. The method includes the steps that vat yellow GOK is dissolved in chloroform and other kinds of halogenated alkane solvent, peroxy-urea is added, the mixed solution is heated to reflux, visible light catalysis is conducted, hydrobromic acid is added dropwise to conduct a bromination reaction, and a reflux reaction continues after hydrobromic acid is added dropwise. A separated vat golden yellow RK product is directly filtered out through aftertreatment, and fresh chloroform and other halogenated alkanes are washed and dried. The method for preparing vat golden yellow RK through oxidative bromination does not use bromine, a green oxidizing agent peroxy-urea and inorganic hydrobromic acid are used as a bromine source, and selectivity is high. The method is easy to operate, reactions are easy to control and short in reaction time, and the process is reliable, clean, free of pollution, high in atom use ratio and suitable for industrial production.

Description

technical field [0001] The invention relates to a method for preparing reduced golden RK by oxidizing bromine, which belongs to the technical field of organic synthesis. Background technique [0002] Vat Golden RK[cas:1324-11-4] is a kind of vat dye, which is used for dyeing cotton products, rayon and rayon, etc., and can also be used for printing. The synthesis method reported in the literature (Handbook of Fine Chemical Products. Dye He Hailan Chief Editor) is: use vat yellow GOK as raw material, add liquid bromine for bromination until the bromine content reaches about 28%. However, during the reaction, controlled fuming sulfuric acid is used as a solvent, sodium nitrite and iodine are used as a catalyst, and liquid bromine is used as a bromination reagent. Bromination is carried out at 85-90 ° C. After the reaction, a large amount of waste acid is produced, which is a risk factor in the operation process. Large, large pollution to the environment, does not meet the requ...

Claims

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Application Information

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IPC IPC(8): C07C45/63C07C49/697
CPCC07C45/63C07C49/697
Inventor 吴孝兰马骏薛循育倪传宏顾金凤
Owner SINOPHARM CHEM REAGENT