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Method for preparing thioamide derivative

A technology for thioamides and derivatives, which is applied in the field of preparing thioamide derivatives, can solve the problems of low yield, limited application of thioamide derivatives, complicated product purification and processing, etc., and achieves high yield and easy operation. , the effect of fewer steps

Active Publication Date: 2015-02-18
心邀(深圳)生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are some improvement means and methods for the deficiencies in this technology, but there are shortcomings such as low yield and cumbersome product purification, which limit the expanded application of thioamide derivatives

Method used

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  • Method for preparing thioamide derivative
  • Method for preparing thioamide derivative
  • Method for preparing thioamide derivative

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Embodiment 1: the synthesis of compound A;

[0030] Add 1.0mmol of 4-methoxybenzaldehyde, 1.2mmol of elemental sulfur, 0.2mmol of DBU and 2.0mL of DMF to the reaction vessel in sequence, and stir the resulting solution in an oil bath at 120°C for 4h, stop heating, and wait for the reaction temperature to drop to After room temperature, add silica gel to the reactant, spin off the solvent after being adsorbed for a certain period of time, and elute and separate the silica gel with the product adsorbed by thin-layer chromatography according to the volume ratio of petroleum ether: ethyl acetate = 10:1 to obtain yellow Crystalline product A, the structure of the compound was confirmed by comparison with known compounds by NMR.

Embodiment 2

[0031] Embodiment 2: the synthesis of compound B;

[0032] Add 1.0mmol of 4-methylbenzaldehyde, 1.2mmol of elemental sulfur, 0.1mmol of DBU and 3.0mL of DMF to the reaction vessel in sequence, and stir the resulting solution in an oil bath at 120°C for 4h, stop heating, and wait for the reaction temperature to drop to room temperature Finally, add silica gel to the reactant, spin off the solvent after being adsorbed for a certain period of time, and elute and separate the silica gel with the product adsorbed by thin layer chromatography according to the volume ratio of petroleum ether: ethyl acetate = 10:1 to obtain yellow crystals Product B, the structure of the compound was confirmed by comparison with known compounds by NMR.

Embodiment 3

[0033] Embodiment 3: the synthesis of compound C;

[0034] Add 1.0mmol of 3-methylbenzaldehyde, 1.3mmol of elemental sulfur, 0.2mmol of DBU and 1.0mL of DMF into the reaction vessel in sequence, and stir the resulting solution in an oil bath at 100°C for 5h, stop heating, and wait for the reaction temperature to drop to room temperature Finally, add silica gel to the reactant, spin off the solvent after being adsorbed for a certain period of time, and elute and separate the silica gel with the product adsorbed by thin layer chromatography according to the volume ratio of petroleum ether: ethyl acetate = 10:1 to obtain yellow crystals Product C, the structure of the compound was confirmed by comparison with known compounds by NMR.

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Abstract

The invention discloses a method for preparing a thioamide derivative. The method comprises the following steps: adding substituted aromatic aldehyde ketone compounds, elemental sulfur, 1,8-diazabicyclo(5.4.0)undec-7-ene and N,N-dimethyl formamide into a reaction container, mixing, and heating and stirring the prepared solution under an oil bath condition; and separating and purifying to obtain the thioamide derivative. The novel method for preparing the thioamide derivative is simple, easily available in raw materials, few in steps, high in yield and friendly to environment, and has a wide application prospect.

Description

technical field [0001] The present invention relates to the technical field of thioamide derivatives, more specifically, to a method for preparing thioamide derivatives. Background technique [0002] Thioamide compounds are an important class of organic compounds, which can be used as intermediates of pharmaceutical compounds and are widely used as inhibitors of biological enzymes in the field of biomedicine. They have unique biological activities and are often used in asymmetric catalysis. In the field of coordination chemistry, thioamide compounds can be used as ligands to design and synthesize complexes with specific functions. In addition, they can also be used to construct electrode materials and functional polymer materials, and have a wide range of applications. [0003] At present, the preparation of thioamide derivatives mainly contains the following two methods: [0004] 1. Reaction of amides with Lawson's reagent or phosphorus pentasulfide; [0005] 2. Willgerod...

Claims

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Application Information

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IPC IPC(8): C07C327/48C07C327/44
Inventor 刘卫兵周鹏陈翠张庆
Owner 心邀(深圳)生物科技有限公司
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