Preparation method of 3,5-dihalobenzotrifluoride and 3'-chloro-5'-(trifluoromethyl)phenyltrifluoroethanone

A technology of dihalotrifluorotoluene and phenyl trifluoroethyl ketone is applied in the field of chemical pharmacy, and can solve the problems of affecting the economic effect of enterprises, increasing the production cost of enterprises, complicated production process and the like, and achieving low price, low production cost, The effect of simple and easy-to-obtain raw materials

Active Publication Date: 2020-12-22
TAIZHOU ABSOBIOTEC CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the production process of 3,5-dihalotrifluorotoluene is relatively complicated and difficult to produce on a large scale, which increases the production cost of the enterprise and seriously affects the economic effect of the enterprise

Method used

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  • Preparation method of 3,5-dihalobenzotrifluoride and 3'-chloro-5'-(trifluoromethyl)phenyltrifluoroethanone
  • Preparation method of 3,5-dihalobenzotrifluoride and 3'-chloro-5'-(trifluoromethyl)phenyltrifluoroethanone
  • Preparation method of 3,5-dihalobenzotrifluoride and 3'-chloro-5'-(trifluoromethyl)phenyltrifluoroethanone

Examples

Experimental program
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Effect test

Embodiment 1

[0049] A method for preparing 3,5-dihalogenobenzotrifluoride, which uses 3,5-dichlorobenzotrifluoride (compound I) as a raw material to prepare compound II through the following steps.

[0050] S1. Dissolve 0.2mol of compound 1 in 200mL of solvent I, and cool down to 0°C to obtain reaction solution I;

[0051] S2. 84g of sulfuric acid with a mass fraction of 92.5% was added dropwise to the reaction solution I, and the dropwise addition process was completed within 30 minutes. After the dropwise addition, the reaction was continued for 1 hour to obtain the reaction solution II;

[0052] S3. Add a nitrous acid reagent solution containing 0.44 mol of nitrous acid reagent to the reaction solution II, keep the temperature of the system below 0° C., and keep the reaction for 2 hours to obtain the reaction solution III;

[0053] S4. The temperature of the reaction solution III was raised to 20°C, and 87 g of 50% hypophosphorous acid was evenly added within 60 minutes, and 0.5 g of cu...

Embodiment 2～6

[0060] A preparation method of 3,5-dihalogenotrifluorotoluene, the difference from Example 1 is that R 1 and R 2 different. R in Examples 2-6 1 and R 2 As shown in Table 1.

[0061]

Embodiment 7～8

[0063] A method for preparing 3,5-dihalogenotrifluorotoluene, the difference from Example 1 is that in step S1, ethanol and isopropanol are selected as solvent I respectively.

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Abstract

The invention relates to the technical field of chemical pharmacy, particularly to a preparation method of 3,5-dihalobenzotrifluoride. According to the preparation method, 3,5-dihalogen-4-amino trifluorotoluene is used as a raw material and is subjected to diazotization deamination reaction to obtain the 3,5-dihalobenzotrifluoride, so that the production cost is relatively low, and the economic effect is relatively good. The invention further relates to a preparation method of 3'-chloro-5'-(trifluoromethyl)phenyltrifluoroethanone. According to the preparation method, 3,5-dihalobenzotrifluorideis used as a raw material, and is subjected to a Grignard reagent reaction, then a nucleophilic addition reaction is carried out with and a trifluoromethylation reagent, and a good economic effect isalso achieved.

Description

technical field [0001] This application relates to the technical field of chemical industry and pharmacy, especially to a preparation method of 3,5-dihalobenzotrifluoride; this application also relates to a 3'-chloro-5'-(trifluoromethyl)phenyltrifluorotoluene The preparation method of fluoroethyl ketone. Background technique [0002] 3-Halo-5-(trifluoromethyl)phenyltrifluoroethanone is an important intermediate used in the synthesis of pesticides or veterinary drugs, and has broad market prospects. [0003] 3,5-Dihalogenotrifluorotoluene is one of the raw materials for the preparation of 3’-chloro-5’-(trifluoromethyl)phenyltrifluoroethanone. At present, the production process of 3,5-dihalotrifluorotoluene is relatively complicated and difficult to produce on a large scale, which increases the production cost of the enterprise and seriously affects the economic effect of the enterprise. Contents of the invention [0004] Aiming at the deficiencies in the prior art, first ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C17/35C07C25/13C07C245/20C07C45/68C07C49/80C07F3/02
CPCC07C17/35C07C245/20C07C45/68C07F3/02C07C25/13C07C49/80Y02P20/55
Inventor 张凌霄蔡刚华
Owner TAIZHOU ABSOBIOTEC CO LTD
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