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Synthesis method of clotrimazole

A synthetic method, the technology of clotrimazole, applied in the field of chemical synthesis, can solve the problems of long production cycle, cumbersome operation, and many wastes, and achieve the effect of simple operation, high reactivity, and environmental friendliness

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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In short, there are many unsafe factors in the current method of synthesizing clotrimazole; and the operation is cumbersome, the cost is high, the yield is low, the three wastes are many, and the production cycle is long

Method used

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  • Synthesis method of clotrimazole
  • Synthesis method of clotrimazole
  • Synthesis method of clotrimazole

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Experimental program
Comparison scheme
Effect test

Embodiment

[0021] A kind of synthetic method of clotrimazole, the steps are as follows:

[0022] Take 4mmol of 2-chlorotrityl chloride, 8mmol of imidazole and 8mmol of sodium carbonate, add 20mL of hexafluoroisopropanol (HFIP), and stir at room temperature (25°C) for 48h. The reaction formula is as follows:

[0023]

[0024] After the reaction was completed, the reaction was determined by TLC, concentrated and separated by column chromatography.

[0025] The reaction yield was detected to be 92%.

[0026] The clotrimazole prepared by the embodiment of the present invention 1 was added in deuterated chloroform (CDCl 3 ), carry out nuclear magnetic resonance analysis, the result is as follows:

[0027] 1HNMR (500MHz, CDCl 3 )δ7.46(s,1H),7.41(d,J=7.7Hz,1H),7.34(d,J=1.2Hz,7H),7.24(d,J=8.0Hz,1H),7.20(d , J=1.3Hz, 4H), 7.06(s, 1H), 6.93(d, J=7.8Hz, 1H), 6.75(s, 1H).

[0028] 13CNMR (125MHz, CDCl 3 )δ 140.90, 140.38, 139.13, 135.59, 132.23, 130.42, 130.19, 129.87, 128.43, 128.17, 128....

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Abstract

The invention discloses a synthesis method of clotrimazole, and belongs to the technical field of chemical synthesis. According to the method, 2-chlorotrityl chloride and imidazole are taken as raw materials, hexafluoroisopropanol is taken as a solvent, and reaction is performed in an alkali environment. The method has the advantages that the raw materials 2-chlorotrityl chloride and imidazole areeasy to get; the reaction can be performed at room temperature, and the reaction condition is mild; other than previous multistep reaction, the method adopts one-step synthesis and is simple to operate; the method is high in reaction activity, the yield reaches 92 percent, and the raw materials are completely converted; products are convenient to separate, and the reaction has green economical efficiency, and is environmentally friendly.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a method for synthesizing clotrimazole. Background technique [0002] Clotrimazole (Clotrimazole) is a synthetic antifungal drug; especially for deep infection of fungi has a high efficacy. The traditional chemical synthesis methods of clotrimazole include: the condensation synthesis method of ester+Grignard reagent and the synthesis method using o-chlorotoluene as raw materials. The total yield of the latter synthetic route is about 32%, and the total yield of the former synthetic route is slightly It is higher than the latter, but there are many unsafe factors in the former synthetic route; the two are cumbersome to operate, low in yield, with many wastes and long production cycle. [0003] On the basis of the above two methods, the methods to improve them are: [0004] Using o-chlorotoluene as raw material, o-chlorotoluene is chlorinated to generate o-...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/56
Inventor 肖建朱帅李帅帅
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