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Preparation method of trifluoroacetophenone derivative

A technology for trifluoroacetophenone and derivatives, which is applied in the field of preparation of trifluoroacetophenone derivatives, can solve the problems of high energy consumption, unsuitability for industrial production, etc. produce less effect

Pending Publication Date: 2021-10-01
TAIZHOU ABSOBIOTEC CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Secondly, the reaction needs to be carried out in the range of minus 80°C, which consumes a lot of energy and is not suitable for industrial production.
[0013] In summary, for the above-mentioned derivatives of trifluoroacetophenone, there is still no relatively suitable industrial production process to produce it

Method used

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  • Preparation method of trifluoroacetophenone derivative
  • Preparation method of trifluoroacetophenone derivative
  • Preparation method of trifluoroacetophenone derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Example 1, a method of preparing a trifluorophenylidene derivative (3,5-dichloro-trifluorophenylidezone), and its reaction formula is shown in formula I-A.

[0049]

[0050] The specific reaction of the reaction includes the steps of:

[0051] S1, weighing compound I0.3 mol (48.6 g), slowly dripping in a 300 g of sulfuric acid solution (containing acid I (sulfuric acid) in 0.61 mol), and then held stirring during the dropwise addition. After completion, stirring was stirred for 20 min, then cooled to -5 ± 5 ° C, and 76 g of a 20% aqueous solution (containing diazotization reagent (sodium nitrite) was added dropwise, and the dropwate was 2 h. After the dropwise addition, the temperature was less than 0 ° C and reacted. After the point plate was monitored until the reactive material point completely disappeared, the reactive nitrogen was obtained, and the atrosity was obtained at 0 ° C.

[0052]S2, 7.5 g of pentaqueous sulfate (inorganic salting catalyst, 0.03 mol), 9.0 g o...

Embodiment 2～17

[0054] Examples 2 to 17, the difference from Embodiment 1 is that the compound I is replaced, and thus, the obtained compound IV has corresponding changes. The amount of the substance to which the compound I was added to the reaction was maintained unchanged, and the other parameters in the reaction were also maintained unchanged, and the yield of the particular compound I and the prepared target product (compound IV) was shown in Table 1.

Embodiment 1～17

[0055] Table 1, Example 1 to 17 Compound yield

[0056]

[0057]

[0058]

[0059] In the above embodiment, the nuclear magnetic resonance spectrum of compound IV in which a part of the compound IV is shown in Table 2.

[0060] Table 2, the structural characterization of partial compounds

[0061]

[0062]

[0063] In the above embodiment, the nuclear magnetic resonance spectrum was determined in deuterated chloroform.

[0064] By the above experimental data, the preparation method in the present application can be used to first achieve a higher reaction yield, and the yield of all reactions is over 65%, and the entire reaction is actually a pot to cook, out In the step S2, there is a step of resetting the liquid, and the remaining time can be carried out in the same reactor, and the subsequent separation is only simply washed, and the solvent is removed. The process required for the reaction process is short, the consumption is less, the condition is mild It is easy to ...

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Abstract

The invention relates to the field of organic synthesis, in particular to a preparation method of a trifluoroacetophenone derivative. Substituted aniline is used as a raw material, and preparation of the trifluoroacetophenone derivative is completed through three steps including diazotization reaction, coupling reaction and hydrolysis reaction. The preparation method has the advantages of simple process, high yield and less three wastes generated by the whole reaction, and is suitable for large-scale industrial production.

Description

Technical field [0001] The present application relates to the field of organic synthesis, and more particularly, it involves a method of preparation of trifluorophenylideophenone derivatives. Background technique [0002] Derivatives of trifluorophenone are an important pharmaceutical intermediate, such as 3,5-dichloroprofluoromethylthrophenone, 3,5-dichloro-4-fluorophenyltone, 3,4,5-Trichloroprofluoromethylthrophenone, 3-chloro-5-trifluoromethyl trifluorophenylideophenide can be used as a synthetic intermediate of a plurality of insecticides. [0003] For trifluorophenylidene derivatives, there are currently several synthetic methods. [0004] 1. Condensation reaction by benzaldehyde with trifluoromethylsilane, preparing trifluorophenylidezone, and specific reactions are shown in formula II. [0005] [0006] In the above reaction, both raw materials are not easy, and the total yield is about 60%, the yield is low, and it is not applicable to industrial production. [0007] 2....

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/51C07C49/80
CPCC07C45/516C07C249/12C07C245/20C07C49/80C07C251/48
Inventor 张凌霄蔡刚华
Owner TAIZHOU ABSOBIOTEC CO LTD
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