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Method used for preparing 2,4-dichloro-5-fluorobenzoyl chloride

A technology of fluorobenzoyl chloride and dichlorofluorobenzene, which is applied in the field of synthesizing 2,4-dichloro-5-fluorobenzoyl chloride with zeolite magnetic composite carrier catalyst, can solve the problem of excessively long process route and the yield of highly toxic chemicals. Difficult to achieve industrial production and other problems, to achieve the effect of facilitating sedimentation growth, improving catalytic activity, and good synergistic effect

Active Publication Date: 2016-06-15
ZHEJIANG YONGTAI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The above existing processes all have problems such as too long process route, use of highly toxic chemicals, yield, etc., making it difficult to realize industrialized production

Method used

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  • Method used for preparing 2,4-dichloro-5-fluorobenzoyl chloride

Examples

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Effect test

preparation example Construction

[0052] Preparation of composite zeolite solid super acid catalyst

[0053] Step (1): Zeolite pretreatment

[0054] A1

[0055] After roasting the mordenite carrier at 450°C, add an ammonium nitrate solution with an ammonium ion concentration of 1.0 mol / L for exchange treatment. The ratio of ammonium salt solution to zeolite liquid solids is 4:1, and the exchange time is 6 hours. Repeat 4 times, wash the exchanged mordenite with deionized water, then dry and calcinate again at 450°C;

[0056] Put the above-mentioned zeolite calcined again into H at a concentration of 6mol / L 2 SO 4 Soaked in the solution for 6 hours, washed with deionized water to neutrality, then dried and calcined at 450°C for 8 hours to obtain the pretreated carrier.

[0057] A2

[0058] After roasting the mordenite carrier at 650°C, add an ammonium sulfate solution with an ammonium ion concentration of 0.05 mol / L for exchange treatment. The ratio of ammonium salt solution to zeolite liquid solids is 3:1, and the excha...

Embodiment 1

[0110] Example 1: Preparation of 2,4-Dichloro-5-fluorobenzotrichloride

[0111] Add 194ml (2mol) of carbon tetrachloride and 33g (0.2mol) of 2,4-dichlorofluorobenzene to a 2L reactor, and then add 50g of the catalyst 8 in Table 1 to the reactor. The reaction is under reflux After reacting for 30 minutes, the reaction mixture was cooled to room temperature and poured into ice water. The organic layer was separated and subjected to chromatographic analysis. It was found that the product contained 94% of 2,4-dichloro-5-fluorobenzotrichloride.

Embodiment 2

[0112] Example 2: Preparation of 2,4-Dichloro-5-fluorobenzoyl chloride

[0113] Add 194ml (2mol) of carbon tetrachloride and 33g (0.2mol) of 2,4-dichlorofluorobenzene to a 2L reactor, and then add 16g of the catalyst 8 in Table 1 to the reactor, and the reaction is under reflux After reacting for 30 minutes, the reactor was cooled to room temperature, 200 ml of deionized water was added to the reaction system, and the reaction was carried out at 40°C for 1 hour. After the reaction, the fraction at 143-144°C (35mmHg) was collected by distillation to obtain 39.1 g Slightly yellow liquid with a yield of 86.0%.

[0114] The mass spectrometry and elemental analysis of the product obtained are as follows:

[0115] Mass spectrum: m / z: 225.92 (100.0%), 227.91 (95.9%), 229.91 (30.6%), 226.92 (7.6%), 228.92 (7.3%), 231.91 (3.3%), 230.91 (2.3%).

[0116] Elemental analysis results: C, 36.97; H, 0.89; Cl, ​​46.76; F, 8.35; O, 7.03. The molecular weight of the product is: 227.44.

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Abstract

The invention relates to a method used for synthesis of 2,4-dichloro-5-fluorobenzoyl chloride and suitable for industrialized production; the method comprises the steps: firstly, with 2,4-dichlorofluorobenzene as a raw material, and in the presence of a composite zeolite solid super acidic catalyst, carrying out a reaction with carbon tetrachloride to obtain 2,4-dichloro-5-fluorotrichlorotoluene, and hydrolyzing to obtain 2,4-dichloro-5-fluorobenzoyl chloride.

Description

[0001] This application is a divisional application of the invention patent application with the application number 201510083439.X, the original application date is February 15, 2015, the publication date is June 10, 2015, and the title of the invention is "a 2,4-two Preparation method of chloro-5-fluorobenzoyl chloride". Technical field [0002] The present invention relates to a method for synthesizing 2,4-dichloro-5-fluorobenzoyl chloride, in particular to a method for using loaded phosphotungstic acid / ZrO 2 A method for synthesizing 2,4-dichloro-5-fluorobenzoyl chloride using a zeolite magnetic composite carrier catalyst. Background technique [0003] The molecular formula of 2,4-dichloro-5-fluorobenzoyl chloride is C 7 H 2 Cl 3 FO, the molecular weight is 227.5, and the CAS number is 86393-34-2. 2,4-Dichloro-5-fluorobenzoyl chloride is generally a colorless or slightly yellow liquid with a boiling point of 143-144°C (35mmHg). It is mainly used as a pharmaceutical intermediate...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C51/58C07C63/70B01J29/80
CPCC07C17/269C07C51/58B01J29/80B01J29/061B01J29/26B01J2229/18B01J2229/37B01J35/33C07C25/13C07C63/70
Inventor 李乙军张星周日喜
Owner ZHEJIANG YONGTAI TECH CO LTD
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