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Preparation method of 4-methylthiazol

A technology of methylthiazole and formamide, which is applied in the field of preparation of 4-methylthiazole, can solve the problems of long reaction route of methylthiazole, complicated reaction and difficult control, and high catalyst production cost, and achieves convenient recovery and reuse, and reaction time. Short, easy-to-use effects

Inactive Publication Date: 2013-08-07
HEILONGJIANG UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The purpose of the present invention is to provide a preparation method for 4-methylthiazole in order to solve the problems of long reaction route, complex reaction and difficult control, high production cost and high yield of using catalysts in the preparation of methylthiazole in the existing method

Method used

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  • Preparation method of 4-methylthiazol
  • Preparation method of 4-methylthiazol
  • Preparation method of 4-methylthiazol

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specific Embodiment approach 1

[0021] Specific embodiment one: the preparation method of the 4-methylthiazole of the present embodiment is carried out according to the following steps:

[0022] 1. Preparation of thioformamide: add formamide to the solvent, add phosphorus pentasulfide under stirring state at room temperature, after the addition is completed, heat up to 45-50°C, react for 2 hours, then cool to room temperature, filter, and collect the filtrate. Obtain the mixed solution containing thioformamide; Wherein, the mass ratio of described solvent and formamide is 1.5~4:1, the mass ratio of described phosphorus pentasulfide and formamide is 1.0~1.1:1, described phosphorus pentasulfide It is added in batches, specifically: weigh phosphorus pentasulfide according to the mass ratio of phosphorus pentasulfide and formamide in the ratio of 1.0 to 1.1:1, add the weighed phosphorus pentasulfide in 8 to 10 batches, add a batch of phosphorus pentasulfide every 20 to 30 minutes, and add a batch of phosphorus pe...

specific Embodiment approach 2

[0024] Embodiment 2: The difference between this embodiment and Embodiment 1 is that the solvent described in step 1 is anhydrous ethylene glycol dimethyl ether or dioxane. Other steps and parameters are the same as those in Embodiment 1.

[0025] The anhydrous ethylene glycol dimethyl ether of the present embodiment adopts phosphorus pentoxide to remove water to obtain anhydrous ethylene glycol dimethyl ether.

specific Embodiment approach 3

[0026] Embodiment 3: This embodiment is different from Embodiment 1 or 2 in that: the temperature in step 1 is raised to 45-50° C., and the reaction is carried out for 2 hours. Other steps and parameters are the same as those in Embodiment 1 or Embodiment 2.

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Abstract

The invention relates to a preparation method of 4-methylthiazol. The invention aims at solving the problem that in the existing method for preparing the methylthiazol, the reaction route is long, the reaction is complicated and not easy to control, the production cost of the used catalyst is high and the yield is high. The preparation method comprises the following steps of A, mixing formamide, anhydrous glycol dimethyl ether and phosphorus pentasulfide, heating the mixture to be reacted at the temperature of 45 to 50 DEG C, and filtering the mixture to obtain thioformamide; B, adding chloroacetone into the thioformamide to be reacted at the temperature of 50 to 60 DEG C, adjusting the pH value to 6 to 7, and cooling, filtering, washing and dehydrating the mixture to obtain the 4-methylthiazol. Raw materials are cheap and easy to obtain, the reaction condition is moderate, the synthesis step is simple, no catalyst is used, no pollution exists, the yield is high, operation is simple and convenient, and the solvent can be recycled. The preparation method is applied to the technical field of chemical industry.

Description

technical field [0001] The invention belongs to the technical field of chemical industry, and in particular relates to a preparation method of 4-methylthiazole. Background technique [0002] In the past ten years, with the improvement of people's living standards, people's quality of life requirements are also improving. 4-Methylthiazole is an important intermediate of medicine, pesticide and spice. Because of its unique aroma, it is widely used in domestic It is widely used in medicine, food, cosmetics and some daily necessities. Due to the secrecy of foreign technology, its domestic production and application are greatly restricted. [0003] [CN101870682] reports, [0004] [0005] , the reaction design is more reasonable, but the reaction route is too long, the reaction conditions are harsh, the yield is 78%-82%, and the industrial production cost is high. [0006] According to [U.S.4111948], [0007] [0008] In this reaction, because the thiol group is very un...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/22
Inventor 白有银周金枝高金胜王子时
Owner HEILONGJIANG UNIV
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