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Method of preparing 2,2'-binitrobibenzil

A technology of dinitrobibenzyl and o-nitrobenzyl chloride is applied in the field of compound preparation, which can solve the problems of non-conformity with green chemistry, difficulty in treating three wastes, low product purity, etc., avoiding product loss and high product yield , the preparation method is simple

Active Publication Date: 2017-10-27
甘肃皓天医药科技有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the shortcomings of this method are: the product purity is low, and the production process consumes a lot of water, the three wastes are difficult to deal with, and the energy consumption is high, which does not conform to the concept of green chemistry.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A. Preparation of supported nano-gold catalyst

[0022] Take a 250ml flask, add 200mg P25 and 5ml 0.01mol / L chloroauric acid aqueous solution, stir evenly, place in ultrasonic for 30min, place on a mechanical stirrer, and stir at a medium speed. Take 100ml of 0.01mol / L sodium borohydride aqueous solution, and slowly add it into the chloroauric acid P25 mixture with a syringe pump at a rate of 30ml / h. After complete addition, turn off the mechanical stirring, let stand overnight, centrifuge, wash with water until neutral, and dry in an oven for later use.

[0023] B. Preparation of 2,2-Dinitrobibenzyl

[0024] Take a 5ml quartz flask, add 5mg supported gold nano-catalyst, 20mg o-nitrobenzyl chloride, 30mg diisopropylethylamine, 3ml dichloromethane, ultrasonically disperse, turn on the halogen lamp, and react for 7h. The catalyst was separated by centrifugation, and the reaction product was collected. The liquid phase was detected by GCMS, and the target product 2,2'...

Embodiment 2

[0026] A. Preparation of supported nano-gold catalyst

[0027] Take 10ml of quartz water-cooled reaction tube, add 200mg of P25 and 5ml of 0.01mol / L chloroauric acid methanol solution, stir evenly, and irradiate with high-pressure mercury lamp for 6h under water-cooling condition, the original light yellow suspension turns into purple, centrifuge to separate Wash with water and ethanol until neutral, and dry in an oven for later use.

[0028] B. Preparation of 2,2-Dinitrobibenzyl

[0029] Take a 5ml quartz flask, add 5mg supported gold nano-catalyst, 20mg o-nitrobenzyl chloride, 28mg diisopropylethylamine, 3ml carbon tetrachloride, ultrasonically disperse, turn on the high-pressure mercury lamp, and react for 5h. The catalyst was separated by centrifugation, and the reaction product was collected. The liquid phase was detected by GCMS, and the target product 2,2'-dinitrobibenzyl accounted for 61%. The catalyst was washed with water and ethanol, and then dried, so it could ...

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Abstract

The invention discloses a method of preparing 2,2'-binitrobibenzil by a catalysis method and a preparation method of a catalyst used by the preparation method. The preparation method of 2,2'-binitrobibenzil comprises the steps of taking ortho-nitrobenzyl chloride as a raw material and methyl chloride as a solvent, adding an amine sacrifice agent, taking a noble metal gold loaded nano titanium oxide carrier as the catalyst, performing a reaction under light irradiation, performing sufficient ultrasonic dispersion prior to the reaction, performing solvent reflux in a reaction process, stirring a reaction system in the reaction process to keep the reaction system in a suspension state, and performing solid-liquid separation after reaction completion to obtain a coupled product, namely 2,2'-binitrobibenzil. The preparation method greatly reduces energy consumption caused by a high temperature in the traditional technology, and avoids cost increase and product loss caused by multi-step and multi-time purification; three wastes generated in a production process are few; a technology is concise; a yield of a product is higher; and a green chemistry concept is met.

Description

technical field [0001] The present invention relates to a preparation method of a compound, especially a preparation method of an intermediate used for antiepileptic drug carbamazepine. Specifically, the present invention relates to a preparation method of 2,2'-dinitrobibenzyl by catalytic method Methods. Background technique [0002] Epilepsy is a chronic neurological disease with a wide range of onset ages, that is, from neonatal stage to old age. Epilepsy has a long course, high unpredictability and suddenness, which seriously affects the daily life and work of patients. Patients and their families often suffer from huge psychological pressure. It is one of the mental diseases that the World Health Organization focuses on prevention and control. According to a joint survey conducted by the Ministry of Health and the China Anti-Epileptic Association, the prevalence of epilepsy in my country is about 7‰, and the prevalence of active epilepsy is about 4.6‰. Therefore, the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C209/68C07C211/50B01J23/52
CPCB01J23/52C07C209/68C07C211/50
Inventor 马建泰骆沙
Owner 甘肃皓天医药科技有限责任公司
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