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Preparation method of halogenated acid compound

A compound and acid technology, which is applied in the field of preparation of halogenated acid compounds, can solve the problems of poor safety and controllability, severe reaction triggering, increased pressure on wastewater treatment, etc., and achieves the effects of low toxicity, high yield, toxicity and environmental protection

Pending Publication Date: 2022-03-25
上海药坦药物研究开发有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, in the reaction process, it is necessary to control the pH value, which is commonly used as hydrochloric acid or phosphate buffered salt. Due to the special properties of this product, the use of hydrochloric acid will produce a large amount of chloride impurities or eliminate impurities. The reaction is violent and the safety controllability is poor. , not conducive to industrial production
The use of phosphate buffer will greatly increase the pressure of wastewater treatment in industrial production

Method used

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  • Preparation method of halogenated acid compound
  • Preparation method of halogenated acid compound
  • Preparation method of halogenated acid compound

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0079] Dissolve 5.9 g of sodium chlorite (52.19 mmol) with a mass fraction of 80% in 18 g of water and set aside.

[0080] Add 8-bromooctyl alcohol 10g (47.82mmol), acetonitrile 39g, water 18g, TEMPO 0.07g (0.45mmol) in the reaction bottle, warm up to 30 ℃, dropwise add 6% sodium hypochlorite aqueous solution 0.5g (0.40mmol), dropwise The sodium chlorite aqueous solution 4.8g (10.48mmol) that has configured, drips and feeds carbon dioxide gas to keep the reaction system at pH=6~7 all the time, after the reaction triggers, keep internal temperature 30 ℃, continue to dropwise add 1.25g ( 1.0mmol) 6% sodium hypochlorite aqueous solution and 19.1g (41.71mmol) of the remaining sodium chlorite aqueous solution prepared. After dropping, the reaction was stirred at 30°C for 2h. Control the temperature below 30°C, add dropwise 20% sodium sulfite aqueous solution to quench the reaction, add 33% dilute sulfuric acid to adjust pH = 3, stand to separate layers, and concentrate the organic...

Embodiment 2

[0083] Dissolve 12g of sodium chlorite (106.15mmol) with a mass fraction of 80% in 40g of water for use.

[0084] Add 20g (95.64mmol) of 8-bromooctyl alcohol, 80g of acetonitrile, 40g of water, 0.15g (0.96mmol) of TEMPO into the reaction flask, raise the temperature to 35°C, add 1g (0.81mmol) of 6% sodium hypochlorite aqueous solution dropwise, and add dropwise to configure 10g (20.41mmol) of a good sodium chlorite aqueous solution, after the dropwise addition of carbon dioxide gas to keep the reaction system at pH = 5 ~ 6, after the reaction is triggered, keep the internal temperature at 35 ° C, continue to drop 2.5g (2.02mmol ) 6% sodium hypochlorite aqueous solution and the remaining sodium chlorite aqueous solution 42g (85.74mmol) configured. After dropping, the reaction was stirred at 35°C for 1h. Control the temperature below 35°C, add 20% sodium sulfite aqueous solution dropwise to quench the reaction, add 33% dilute sulfuric acid to adjust pH = 2, let stand to separat...

Embodiment 3

[0086] Dissolve 1.2 kg of sodium chlorite (10.61 mol) with a mass fraction of 80% in 4 kg of water and set aside.

[0087] 2kg (9.6mol) of 8-bromooctyl alcohol, 8kg of acetonitrile, 4kg of water, TEMPO14.7g (0.094mol) were added to the 50L reactor, and the temperature was raised to 20°C, and 100g (0.08mol) of 6% sodium hypochlorite aqueous solution was added dropwise. 1 kg (2.04 mol) of the prepared sodium chlorite aqueous solution, after the dropwise feeding of carbon dioxide gas to keep the reaction system at pH = 5 ~ 6, after the reaction is triggered, keep the internal temperature at 20 ° C, continue to drop 250 g (0.20 mol ) 6% sodium hypochlorite aqueous solution and 4.2kg (8.57mol) of the remaining sodium chlorite aqueous solution configured. After dropping, the reaction was stirred at 20°C for 1.5h. Control the temperature below 20°C, add 20% sodium sulfite aqueous solution dropwise to quench the reaction, add 33% dilute sulfuric acid to adjust pH = 3, stand to separa...

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Abstract

The invention discloses a preparation method of a halogenated acid compound. Specifically, the invention provides a preparation method of a halogenated acid compound as shown in a formula I. A halogenated alcohol compound as shown in a formula II is taken as a raw material and reacts with TEMPO, sodium hypochlorite and sodium chlorite, the reaction pH is regulated by carbon dioxide which is low in cost and easy to obtain, and finally the halogenated acid compound is prepared. The preparation method is high in yield, relatively low in toxicity, environment-friendly and suitable for industrial production.

Description

technical field [0001] The invention relates to a preparation method of halogenated acid compounds. Background technique [0002] As an excellent pharmaceutical and pesticide intermediate, 8-bromooctanoic acid has the following structure: [0003] [0004] Regarding the synthesis of 8-bromooctanoic acid, there are relatively few methods, and the more conventional ones are as shown in patent CN113087623: 1,6-dibromohexane is used as the main raw material to carry out substitution reaction with diethyl malonate, and then hydrolyzed by ester group And decarboxylation to obtain 8-bromooctanoic acid. The reaction time of this route is long, the conversion rate of the first step is low, the temperature of the decarboxylation reaction is high, and there are many by-products. At the same time, in order to increase the selectivity of the first step of substitution, the raw material 1,6-dibromohexane is greatly excessive. [0005] Route 1: [0006] [0007] Refer to J.Org.Che...

Claims

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Application Information

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IPC IPC(8): C07C51/295C07C51/43C07C51/44C07C53/19
CPCC07C51/295C07C51/44C07C51/43C07C53/19
Inventor 陈晓冬刘冰辉洪辉意褚长虎刘学军
Owner 上海药坦药物研究开发有限公司
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