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A kind of preparation method of 2,4-dichloro-5-fluorobenzoyl chloride

A technology of fluorobenzoyl chloride and dichlorofluorobenzene is applied in the field of synthesizing 2,4-dichloro-5-fluorobenzoyl chloride with a zeolite magnetic composite carrier catalyst, which can solve the problem that it is difficult to realize industrialized production, and the process route is too long and highly toxic Chemical yield and other issues, to achieve the effect of improving catalytic activity, facilitating sedimentation growth, and reducing cost of use

Active Publication Date: 2017-12-08
ZHEJIANG YONGTAI TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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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  • A kind of preparation method of 2,4-dichloro-5-fluorobenzoyl chloride

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Effect test

preparation example Construction

[0052] Preparation of Composite Zeolite Solid Superacid 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 1.0mol / L for exchange treatment. The volume ratio of ammonium salt solution to zeolite liquid to solid is 4:1, and the exchange time is 6 hours. Repeat 4 times, wash the exchanged mordenite with deionized water, then dry it and bake it again at 450°C;

[0056] Put the aforementioned zeolite that has been roasted again into H2 with a concentration of 6mol / L 2 SO 4 Soak in the solution for 6 hours, wash with deionized water until neutral, dry, and bake at 450° C. for 8 hours to obtain a pretreated carrier.

[0057] A2

[0058] After roasting the mordenite carrier at 650°C, add an ammonium sulfate solution with an ammonium ion concentration of 0.05mol / L for exchange treatment. The volume ratio of ammonium salt solution to zeolite liqui...

Embodiment 1

[0110] Embodiment 1: Preparation of 2,4-dichloro-5-fluorobenzotrichloride

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

Embodiment 2

[0112] Embodiment 2: Preparation of 2,4-dichloro-5-fluorobenzoyl chloride

[0113] In the reactor of 2L, add 194ml (2mol) carbon tetrachloride and 33 grams (0.2mol) 2,4-dichlorofluorobenzene, then add catalyzer 8 in 16 grams of aforementioned Table 1 in reactor, react at reflux The reaction was carried out at room temperature for 30 minutes, then the reactor was cooled to room temperature, 200 milliliters 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. (35 mmHg) was collected by distillation to obtain 39.1 grams Light yellow liquid, yield 86.0%.

[0114] The resulting product was subjected to mass spectrometry and elemental analysis, and the results were 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;...

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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, and the publication date is June 10, 2015. The invention name is "a 2,4-two Preparation method of chloro-5-fluorobenzoyl chloride". technical field [0002] The invention relates to a method for synthesizing 2,4-dichloro-5-fluorobenzoyl chloride, in particular to a method using loaded phosphotungstic acid / ZrO 2 A method for the synthesis of 2,4-dichloro-5-fluorobenzoyl chloride over a zeolite magnetic composite support catalyst. Background technique [0003] The molecular formula of 2,4-dichloro-5-fluorobenzoyl chloride is C 7 h 2 Cl 3 FO, molecular weight 227.5, CAS number 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 for the synthesis of bro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C51/58C07C63/70B01J29/80
CPCB01J29/061B01J29/26B01J29/80B01J35/0033B01J2229/18B01J2229/37C07C17/269C07C51/58C07C25/13C07C63/70
Inventor 李乙军张星周日喜
Owner ZHEJIANG YONGTAI TECH CO LTD
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