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Method for preparing 2-chloro-5-chloromethylthiazole by jet loop reactor

A loop reactor, chloromethylthiazole technology, applied in organic chemistry and other directions, can solve the problems of high reaction temperature control requirements, complex production process, many side reactions, etc., and achieves wide reaction temperature range, high yield, and side reactions. less reactive effect

Active Publication Date: 2016-01-20
河北德瑞化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the production process is complicated and the cost is high
[0008] All there are some deficiencies more or less in the above-mentioned reaction, for example: 1-isothiocyanato-2-propene chlorination method, side reaction is more in the reaction process, simultaneously, very high to the control requirement of reaction temperature, and , during the reaction process, a large amount of heat is released, which is difficult to control in the industrial production process

Method used

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  • Method for preparing 2-chloro-5-chloromethylthiazole by jet loop reactor

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A method utilizing a jet loop reactor to prepare 2-chloro-5-chloromethylthiazole, comprising the following steps:

[0032] 1. Using a jet loop reactor, see figure 1 As shown, the jet loop reactor includes a reactor 1, an injector 2, an air intake pipe 3, a heat exchanger 4 and a circulation pump 5, the injector 2 is installed on the upper part of the reactor 1, and the outlet of the lower part of the reactor 1 passes through a pipeline and a circulation pump 5. The inlet of the pump 5 is connected, the outlet of the circulating pump 5 is connected with the inlet of the heat exchanger 4 through a pipe, the outlet of the heat exchanger 4 is connected with the top inlet of the ejector 2 through a pipe, and the side of the ejector 2 is provided with an inlet Trachea 3, air intake pipe 3 is provided with intake valve. The injector 2 is a jet-type Venturi injector. The heat exchanger 4 is a jacketed tank heat exchanger.

[0033] Two, 1-isothiocyanato-2-chloro-2-propene is ...

Embodiment 2

[0036] A method utilizing a jet loop reactor to prepare 2-chloro-5-chloromethylthiazole, comprising the following steps:

[0037] 1. A jet loop reactor is adopted. The difference between the jet loop reactor and Example 1 is that the heat exchanger 4 is a plate heat exchanger.

[0038] 2. Dissolve 1-isothiocyanato-2-chloro-2-propene in 1,2-dichloroethane to form a liquid phase material with a mass concentration of 40%, add it to reaction kettle 1, and start the cycle Pump 5, the liquid phase material is pressurized by the circulating pump 5, heat exchanged by the heat exchanger 4 to control the temperature, and enters from the top inlet of the injector 2; the intake valve is opened, and the gaseous chlorine gas enters the injector 2 and the liquid phase material through the intake pipe 3 Mix and react, the mixed and reacted materials pass through the reactor 1, the circulation pump 5, the heat exchanger 4 and then return to the top inlet of the injector 2, and circulate the re...

Embodiment 3

[0041] A method utilizing a jet loop reactor to prepare 2-chloro-5-chloromethylthiazole, comprising the following steps:

[0042] 1. A jet loop reactor is adopted. The difference between the jet loop reactor and Embodiment 1 is that the heat exchanger 4 is a tube-and-tube heat exchanger.

[0043] 2. Dissolve 1-isothiocyanato-2-chloro-2-propene in dichloromethane to form a liquid phase material with a mass concentration of 70%, add it to the reaction kettle 1, open the circulation pump 5, and the liquid phase The material is pressurized by the circulation pump 5, heat exchanged by the heat exchanger 4 to control the temperature, and enters from the top inlet of the injector 2; the intake valve is opened, and the gaseous chlorine enters the injector 2 through the intake pipe 3 to mix and react with the liquid phase material. The mixed and reacted materials pass through the reactor 1, the circulation pump 5, and the heat exchanger 4, and then return to the top inlet of the ejecto...

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Abstract

The invention discloses a method for preparing 2-chloro-5-chloromethylthiazole by a jet loop reactor, and relates to the technical field of synthesis of the 2-chloro-5-chloromethylthiazole. The jet loop reactor comprises an ejector, wherein the ejector is arranged at the upper part of the reaction kettle; a lower outlet of the reaction kettle is communicated with an inlet of a circulating pump; an outlet of the circulating pump is communicated with the inlet of a heat exchanger; the outlet of the heat exchanger is communicated with the top inlet of the ejector; an air inlet pipe is arranged on the side surface of the ejector; 1-isothiocyano-2-chlorine-2-propylene is dissolved into an inert organic solvent to prepare a liquid-phase material; the liquid-phase material is added to the reaction kettle, and enters from the top inlet of the ejector after passing through the circulating pump and the heat exchanger; chlorine enters the ejector through the air inlet pipe and is mixed with the liquid-phase material; the mixed material passes through the reaction kettle, the circulating pump and the heat exchanger and then returns to the top inlet of the ejector; circular reaction is carried out until the chlorine is introduced; a 2-chloro-5-chloromethylthiazole product is obtained after post-treatment. The method disclosed by the invention is high in yield, few in solid wastes and high in production efficiency; the reaction temperature is easy to control.

Description

technical field [0001] The invention relates to the technical field of 2-chloro-5-chloromethylthiazole synthesis. Background technique [0002] 2-Chloro-5-chloromethylthiazole (2-Chloro-5-chloromethylthiazole) is an important intermediate in the production of thiamethoxam, clothianidin, dinotefuran and pharmaceutical products. [0003] According to documents described in CN00811445, CN01809972, CN96117934, CN97109983, CN200410056641, CN200780002281, CN201410045648, CN201410045781, CN201410098099-2, CN201410308830, etc. At present, there are many ways to synthesize 2-chloro-5-chloromethylthiazole, which are mainly divided into the following types according to the different raw materials used: [0004] (1) 1-isothiocyanato-2-propene chlorination method: inject chlorine gas (or a compound that can generate chlorine gas, such as sulfuryl chloride) and 1-isothiocyanato-2-propene in chloroform at the same time React in refluxed chloroform. This reaction requires a large amount ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D277/32
CPCC07D277/32
Inventor 宋建华史三冬柳海营周梁
Owner 河北德瑞化工有限公司
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