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Method for recovering 7-chloroquinaldine mother liquor

A technology of mother liquor recovery and pyridine mother liquor, which is applied in the field of medicine and chemical industry, can solve problems such as increased production costs, environmental pollution, and waste of resources, and achieve the effects of avoiding pollution, solving equipment corrosion, and simple processes

Pending Publication Date: 2022-06-17
JIANGSU ALPHA PHARM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But in the reaction process, tetrachloro-p-benzoquinone itself can be reduced to the hydroquinone of complete reduction state, and in actual industrial production, hydroquinone is mostly directly discarded and thrown away, and this not only can make production cost increase, causes resource waste, and will cause serious environmental pollution

Method used

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  • Method for recovering 7-chloroquinaldine mother liquor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 4g of tetrachlorohydroquinone, measure 40mL of benzene, 2mL of concentrated hydrochloric acid, and then weigh 0.04g of CuCl 2 ·2H 2 O or anhydrous CuCl 2 Put them into a three-necked flask together, measure 20 mL of hydrogen peroxide in a constant pressure funnel, and control the dropping rate of hydrogen peroxide, 3s / d, and a reaction temperature of 50 °C. After the reaction for 2.5 hours, the first suction filtration was added, and 15mL distilled water. Continue to stir and mix for 5 min, transfer to a separatory funnel, stand for stratification, take the upper layer liquid in a three-necked flask, and conduct distillation, the obtained fraction is benzene, and the fraction is collected. When about 2-3 mL of the solution remained, pour it out and cool to crystallize. After the crystals were precipitated, the crystals were washed with 2 mL of distilled water, suction filtration was performed for the second time, and the obtained crystals were naturally air-dri...

Embodiment 2

[0020] Weigh 4g of tetrachlorohydroquinone, weigh 30mL of toluene, 2mL of concentrated hydrochloric acid, and weigh 0.04g of CuCO 3 Put them into a three-necked flask together, measure 24 mL of hydrogen peroxide into a constant pressure funnel, and control the dropping rate of hydrogen peroxide at the same time, 3s / d, and the reaction temperature is 45 °C. Distilled water. Continue to stir and mix for 5 min, transfer to a separatory funnel, stand for stratification, take the upper layer liquid in a three-necked flask, and conduct distillation, the obtained fraction is benzene, and the fraction is collected. When about 2-3 mL of the solution remained, pour it out and cool to crystallize. After the crystals were precipitated, the crystals were washed with 2 mL of distilled water, suction filtration was performed for the second time, and the obtained crystals were naturally air-dried. The obtained tetrachlorobenzoquinone yield was 95.9%.

Embodiment 3

[0022] Weigh 4g of tetrachlorohydroquinone, weigh 35mL of methanol, 2mL of concentrated hydrochloric acid, and weigh 0.04g of Cu(OH) 2 Put them into a three-necked flask together, measure 20 mL of hydrogen peroxide in a constant pressure funnel, and control the dropping rate of hydrogen peroxide at the same time, 3s / d, and the reaction temperature is 60 °C. Distilled water. Continue to stir and mix for 5 min, transfer to a separatory funnel, stand for stratification, take the upper layer liquid in a three-necked flask, and conduct distillation, the obtained fraction is benzene, and the fraction is collected. When about 2-3 mL of the solution remained, pour it out and cool to crystallize. After the crystals were precipitated, the crystals were washed with 2 mL of distilled water, suction filtration was performed for the second time, and the obtained crystals were naturally air-dried. The obtained tetrachlorobenzoquinone yield was 95.5%.

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Abstract

The invention belongs to the field of pharmaceutical chemicals, and particularly relates to a method for recovering 7-chloroquinaldine mother liquor. The method mainly comprises the following steps: reacting tetrachloroquinone serving as a raw material and hydrogen peroxide serving as an oxidizing agent in the presence of a copper catalyst under an acidic condition, and performing simple filtering operation and separation to obtain a product chloranil, so as to realize regeneration of chloranil. The method for regenerating the chloranil is relatively low in cost, simple and convenient in post-treatment, relatively high in yield of the chloranil, capable of recycling the solvent for multiple times, simple to operate, less in generated sewage, green and environment-friendly, and suitable for industrial large-scale production.

Description

technical field [0001] The invention belongs to the field of medicine and chemical industry, and in particular relates to a method for recovering a 7-chloroquinalidine mother liquor. Background technique [0002] 7-Chloroquinaldine, chemical name 2-methyl-7-chloroquinaldine, English name 7-chloroquinaldine, CAS No.: 4965-33-7, its chemical structural formula: . As an important pharmaceutical intermediate, 7-chloroquinalidine is mainly used to prepare the important intermediate of antiasthmatic drug montelukast and leukotriene receptor antagonist MK-0679. The traditional method uses m-chloroaniline and crotonaldehyde as the main raw materials to prepare through the classic Skraup reaction and DeobnerMiller reaction. Since the reaction has 5-position isomers, it is necessary to use ZnCl2, tartaric acid or 4-nitrophthalic acid and isomerization. It is separated and purified by the mixed complexation reaction to obtain high-purity 7-chloroquinalidine, so the yield is low. Pa...

Claims

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Application Information

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IPC IPC(8): C07C46/06C07C46/10C07C50/24
CPCC07C46/06C07C46/10C07C2601/16C07B2200/13C07C50/24
Inventor 石利平叶金星陈本顺李大伟徐春涛何义朱萍王欢张维冰马骧钱若灿
Owner JIANGSU ALPHA PHARM CO LTD
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